CN107631918B - Black powder pretreatment method - Google Patents

Black powder pretreatment method Download PDF

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CN107631918B
CN107631918B CN201710651074.5A CN201710651074A CN107631918B CN 107631918 B CN107631918 B CN 107631918B CN 201710651074 A CN201710651074 A CN 201710651074A CN 107631918 B CN107631918 B CN 107631918B
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black powder
liquid
reinforcing agent
treatment
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CN107631918A (en
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粟勇
袁丁
蒋剑
汪强
吴红彦
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Beijing Htnova Detection Technology Co ltd
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Abstract

The invention discloses a pretreatment method of black powder and analogues thereof, which comprises the steps of treating the black powder and the analogues thereof by using a treatment fluid to obtain a sample fluid, using the sample fluid for laser excitation spectrum detection, and obtaining component detection conditions of the black powder and the analogues thereof through the detection of the sample fluid, wherein the use mode of the sample fluid comprises direct use, concentrated use or use after dropwise adding the sample fluid to a test piece to remove a solvent. The method can not only overcome the problem that the black powder and the like are inflammable, but also greatly enhance the laser excitation spectrum signal of the black powder, provide possibility for realizing safe and rapid detection of the black powder, have wide detection components and provide convenience for dangerous object investigation and identification work.

Description

Black powder pretreatment method
Technical Field
The invention relates to a pretreatment method for spectrum detection, in particular to a pretreatment method for black powder and analogues thereof.
Background
At present, the application of laser excitation spectroscopy technology to the detection of dark substances is always a difficult problem in the industry, especially the detection of dark inflammable substances. The main reasons for this technical problem are: when the laser irradiates dark substances, the heat is easy to absorb, and the heat is difficult to diffuse in time after the heat is absorbed, so that the heat accumulation is easy to cause, especially when the laser excitation spectrum technology is used for directly testing dark inflammable substances such as black powder, the danger of combustion and even explosion exists.
On the other hand, the black powder and the like are multi-substance mixed samples, most of the substances are black inflammable substances, only a small amount of components have laser Raman and laser excitation plasma signals, and the signals are weak and are not suitable for direct test by a laser excitation spectrum technology, so that in order to meet the requirement of rapid detection of the black powder and the like, the black powder and the like are preprocessed by adopting a proper means and then detected by using corresponding equipment.
For example, in the article of application of raman spectroscopy technology to explosive detection, raman spectroscopy detection is performed on 12 explosives in the mainstream, detection is successfully completed on the 11 explosives except for black powder, a corresponding spectrum is obtained, the raman spectrum cannot be detected by the black powder with laser power of 50mW and 150mW, and combustion occurs in the detection process with the laser power of 300 mW. Therefore, the problem that the laser excitation spectrum technology in the prior art cannot be directly used for testing black powder needs to be solved urgently.
Disclosure of Invention
The present invention is directed to solving the problems described above. The invention aims to provide a detection pretreatment method suitable for black powder and analogues thereof, which can not only overcome the problem of flammability of the black powder, but also separate substances with laser excitation spectrum scattering characteristics, even enhance the laser excitation spectrum signals of the black powder, and provide possibility for realizing safe and rapid detection of the black powder.
The invention provides a pretreatment method of black powder and analogues thereof, which comprises the steps of treating the black powder and the analogues thereof by using a treatment fluid to obtain a sample fluid, and using the sample fluid for laser excitation spectrum detection, wherein the use mode of the sample fluid comprises direct use, concentrated use or use after dropwise adding the sample fluid to a test piece to remove a solvent; wherein, the process of preparing the sample liquid comprises the following steps:
mixing: fully dissolving the black powder and the analogues thereof by using the treatment fluid to prepare a mixed solution;
deslagging: removing the precipitate in the mixed solution to obtain a sample solution;
the treatment liquid in the mixing step comprises a dispersion liquid and a reinforcing agent, the reinforcing agent in the treatment liquid accounts for 0-10% by mass, and the dispersion liquid is a polar solution comprising water.
Wherein, the reinforcing agent is a cyclic ether compound or a mixture thereof.
The treatment fluid further comprises an acidizing fluid, wherein the acidizing fluid is one or more of a hydrochloric acid solution, a sulfuric acid solution and a nitric acid solution, and the acidizing fluid accounts for 0-10% of the treatment fluid in percentage by mass.
The treatment fluid further comprises an acidizing fluid, wherein the acidizing fluid is selected from a hydrochloric acid solution with the volume concentration of 2-5%, a sulfuric acid solution with the volume concentration of 8-12% or a nitric acid solution with the volume concentration of 4-9%.
Wherein the acidizing fluid is selected from the group consisting of: a hydrochloric acid solution with the volume concentration of 2-5%, wherein the addition amount is 4-6%; or 1-4% of sulfuric acid solution with volume concentration of 8-12%; or 4-6% of nitric acid solution with volume concentration of 4-9%.
Wherein the dispersion further comprises one or more of methanol, ethanol, acetonitrile and acetone.
Wherein the dispersion liquid is selected from water, a water/ethanol mixed solution with a volume ratio of 1: 0.1-0.5 or a water/acetone mixed solution with a volume ratio of 1: 0.2-0.8.
Wherein the reinforcing agent is one or more of crown ether and crown ether derivatives.
Wherein the crown ether and crown ether derivatives comprise 12-crown-4 and derivatives thereof, 15-crown-5 and derivatives thereof, 18-crown-6 and derivatives thereof, 21-crown-7 and derivatives thereof, 24-crown-8 and derivatives thereof, and 30-crown-10 and derivatives thereof.
Wherein the reinforcing agent is a mixture of a reinforcing agent A and a reinforcing agent B, and the reinforcing agent A is selected from 18-crown-6 or a derivative thereof; the reinforcing agent B is selected from 15-crown-5 or derivatives thereof.
Wherein, the mixing step comprises one or more methods of stirring, shaking, ultrasound and heating, and the deslagging step comprises a filtering or centrifuging method.
Wherein the enhancing agent A is
Figure GDA0002618362140000031
Wherein R is1、R2、R3And R4Is H or an electron-donating group, e.g. -OH, -NH2Etc. R1And R2And R3And R4May also be present together in a ring, for example, the enhancing agent A is benzo-18-crown-6.
Wherein the enhancing reagent B is
Figure GDA0002618362140000032
Wherein R is1、R2、R3And R4Is H or an electron-donating group, e.g. -OH, -NH2Etc. R1And R2And R3And R4They may also be present together in a ring, for example, the reinforcing agent B is benzo-15-crown-5.
Wherein the mass ratio of the reinforcing reagent A to the reinforcing reagent B is 1-4: 1.
The pretreatment method also comprises the step of preparing a treatment solution, and the pretreatment method comprises the following specific steps:
preparing a treatment liquid, wherein the treatment liquid comprises a dispersion liquid, an acidizing liquid and an intensifier, and the dispersion liquid is water, a water/ethanol mixed liquid or a water/acetone mixed liquid; adding an acidizing fluid for acidizing, wherein the acidizing fluid is a hydrochloric acid solution, a sulfuric acid solution or a nitric acid solution; finally adding a reinforcing agent, wherein the reinforcing agent is one or more of crown ether and crown ether derivatives;
preparing a sample solution, and treating the black powder and the analogues thereof by using a treatment solution to obtain the sample solution;
the sample liquid is used for laser excitation spectrum detection, and the use mode of the sample liquid comprises direct use, concentration use or use after dropping the sample liquid to a test piece and removing a solvent.
In the step of preparing the treatment solution, the crown ether and the crown ether derivatives comprise 12-crown-4 and derivatives thereof, 15-crown-5 and derivatives thereof, 18-crown-6 and derivatives thereof, 21-crown-7 and derivatives thereof, 24-crown-8 and derivatives thereof, and 30-crown-10 and derivatives thereof, and the addition amount of the reinforcing agent is 0.001-8%.
Wherein, the test piece comprises a glass slide, a glass sheet, test paper, a metal sheet or a plastic sheet.
Wherein the solvent removing method comprises air drying, vacuum drying, freeze drying, heating drying, natural air drying, hot air drying or cold air drying.
The black powder analogue refers to a substance which is dark to black in color, is easy to ignite by laser under a dry condition and is not suitable for laser excitation spectrum detection, and comprises ignition powder, whip powder, gunpowder for paradise, and priming powder.
Wherein the laser excitation spectrum detection comprises laser excitation Raman detection or laser excitation plasma detection.
The detection components of the black powder and the analogues thereof comprise one or more of nitrates such as potassium nitrate, ammonium nitrate and sodium nitrate, chlorates such as potassium perchlorate, sodium perchlorate and ammonium perchlorate, and chlorates such as potassium chlorate, sodium chlorate and ammonium chlorate.
The invention provides a pretreatment method of black powder and analogues thereof, which is characterized in that the black powder and the analogues thereof are mixed with a specially prepared treatment solution, the treatment solution can dissolve substance components with laser excitation spectrum signal characteristics in a mixture, then a sample solution is further obtained by adopting a filtering or centrifuging mode, the sample solution is a transparent or semitransparent solution, and then the component detection condition of the black powder and the analogues thereof is obtained by detecting the sample solution.
The treatment process is combined with the treatment solution, so that the detection components of the black powder and the like can be effectively extracted, and the rapid detection of the laser excitation spectrum is facilitated. The composition and preparation of the treatment solution are the key points of the invention, and the treatment solution has the functions of dissolution, extraction, enhancement and the like.
Specifically, the treatment solution comprises a dispersion liquid and a reinforcing agent, the reinforcing agent in the treatment solution accounts for 0-10% by mass, and the dispersion liquid is a polar solution containing water. The polar solution of the invention refers to a solution with asymmetric molecular structure, and the dispersion liquid can be an aqueous solution or an aqueous solution with polar molecules as solute. When the dispersion is an aqueous solution containing polar molecules, preferably, the aqueous solution of the dispersion further comprises one or more of methanol, ethanol, acetonitrile, and acetone. The main function of the dispersion liquid is to disperse the acidizing fluid and the strengthening agent and dissolve and extract the detection components of the black powder and the like.
It can be understood that when the addition amount of the reinforcing agent is zero, the dispersion can realize the dissolution and extraction of the detection component, and has a basic pretreatment effect. More preferably, the dispersion is selected from water, a water/ethanol mixed solution with a volume ratio of 1: 0.1-0.5 or a water/acetone mixed solution with a volume ratio of 1: 0.2-0.8, and the three dispersions have excellent pretreatment effects.
As an innovative point of the invention, the treatment fluid comprises an enhancer which is a cyclic ether compound or a mixture thereof. The reinforcing agent has the main function of reinforcing the laser excitation spectrum signal of the detected component in the sample liquid, so that better pretreatment effect is realized.
The cyclic ether compound of the present invention refers to cyclic ethers and substituted cyclic ether derivatives. Preferably, the enhancer is one or more of a crown ether and a crown ether derivative; wherein, crown ether refers to a crown ether containing a plurality of-OCH in the molecule2CH2-macrocyclic polyethers of structural units. Preferably, the crown ethers and crown ether derivatives include 12-crown-4 and derivatives thereof, 15-crown-5 and derivatives thereof, 18-crown-6 and derivatives thereof, 21-crown-7 and derivatives thereof, 24-crown-8 and derivatives thereof, 30-crown-10 and derivatives thereof.
The invention has conducted a great deal of research on a dispersion liquid system, and the treatment liquid of the invention has a reinforcing agent content of 0 to 10% by mass, preferably 0.001 to 8% by mass, more preferably 0.01 to 5% by mass, and has a superior reinforcing effect.
Preferably, the enhancer is a mixture of enhancer agent a and enhancer agent B, which are different crown ethers or crown ether derivatives. In some examples of the invention, most preferably, the enhancing agent a is selected from 18-crown-6 or a derivative thereof and the enhancing agent B is selected from 15-crown-5 or a derivative thereof. More preferably, the mass ratio of the reinforcing agent A to the reinforcing agent B is 1-4: 1, and the reinforcing agent has a better beneficial effect.
The treatment fluid also comprises an acidizing fluid, and the acidizing fluid has the main functions of being matched with the dispersion fluid and the reinforcing agent, enhancing the dissolving and extracting functions and the signal enhancing function of the treatment fluid, realizing better pretreatment effect and simultaneously improving the stability of the reinforcing agent in the treatment fluid. The acidizing fluid comprises one or more of a hydrochloric acid solution, a sulfuric acid solution and a nitric acid solution, and the mass percentage of the acidizing fluid in the treatment fluid is 0-10%.
Preferably, the acidizing fluid is selected from a hydrochloric acid solution with a volume concentration of 2-5%, a sulfuric acid solution with a volume concentration of 8-12% or a nitric acid solution with a volume concentration of 4-9%. More preferably, the acidifying liquid is selected from: a hydrochloric acid solution with the volume concentration of 2-5%, wherein the addition amount is 4-6%; or 1-4% of sulfuric acid solution with volume concentration of 8-12%; or 4-6% of nitric acid solution with volume concentration of 4-9%.
Most preferably, the acidified liquid is selected from: 3.6 percent of hydrochloric acid solution with the volume concentration, and the adding amount is 5 percent; or a sulfuric acid solution with the volume concentration of 10 percent, and the adding amount is 2 percent; or 6.7 volume percent nitric acid solution, and the addition amount is 5 percent.
A large number of tests and application data prove that the treatment liquid provided by the invention, for example, the reinforcing agent is a cyclic ether compound, the acidizing liquid comprises one or more of a hydrochloric acid solution, a sulfuric acid solution and a nitric acid solution, the dispersion liquid is a polar solution comprising water, and the treatment liquid prepared by the optimized composition and the optimized content has good pretreatment effect, so that the safe and rapid test of the laser excitation spectrum technology for black powder and the like can be facilitated.
As an innovative point of the present invention, the pretreatment method includes a preparation step of treatment, and the pretreatment method includes the following steps:
preparing a treatment solution, and sequentially adding an acidizing solution and a reinforcing agent into the dispersion solution according to the proportion of the treatment solution; treating the black powder and the like by using a treatment fluid to obtain a sample fluid; the sample liquid is used for laser excitation spectrum detection, and the use mode of the sample liquid comprises direct use, concentration use or use after dropwise adding the sample liquid to a test piece and removing a solvent.
The treatment process of the treating fluid and the black powder and the like in the present invention includes all methods for mixing and dissolving the sample, such as stirring, shaking, ultrasonic, heating and combination thereof.
The sample liquid can be directly used for laser excitation spectrum detection or used for laser excitation spectrum detection after the solvent is concentrated, and the sample liquid can also be dropwise added to a test piece to remove the solvent to obtain solid crystals for laser excitation spectrum detection. The test piece includes a carrier which can be used for a removing process such as solvent volatilization, and the like, such as a glass slide, a glass sheet, test paper, a metal sheet or a plastic sheet, and the like, but is not limited thereto; the solvent may be removed by air drying, vacuum drying, freeze drying, heat drying, natural air drying, hot air drying or cold air drying, but is not limited thereto.
As a preferable example of the present invention, the pretreatment method includes the steps of:
preparing a treatment liquid, wherein the treatment liquid comprises a dispersion liquid, an acidizing liquid and an intensifier, and the dispersion liquid is water, a water/ethanol mixed liquid or a water/acetone mixed liquid; adding an acidizing fluid for acidizing, wherein the acidizing fluid is a hydrochloric acid solution, a sulfuric acid solution or a nitric acid solution; finally adding a reinforcing agent, wherein the reinforcing agent is one or more of crown ether and crown ether derivatives;
preparing a sample solution, and treating the black powder and the analogues thereof by using a treatment solution to obtain the sample solution;
the sample liquid is used for laser excitation spectrum detection, and the use mode of the sample liquid comprises direct use, concentration use or use after dropping the sample liquid to a test piece and removing a solvent.
As another preferable example of the present invention, the pretreatment method includes the steps of:
preparing a treatment liquid, wherein the treatment liquid comprises a dispersion liquid, an acidizing liquid and an enhancer, and the dispersion liquid is selected from water, a water/ethanol mixed solution with a volume ratio of 1: 0.1-0.5 or a water/acetone mixed solution with a volume ratio of 1: 0.2-0.8; adding an acidizing fluid for acidizing, wherein the acidizing fluid is selected from the group consisting of: a hydrochloric acid solution with the volume concentration of 2-5%, wherein the addition amount is 4-6%; or 1-4% of sulfuric acid solution with volume concentration of 8-12%; or 4-6% of nitric acid solution with volume concentration of 4-9%; finally, adding a reinforcing agent, wherein the reinforcing agent is one or more of crown ether and crown ether derivatives, and the adding amount of the reinforcing agent is 0-5%;
preparing a sample solution, and treating the black powder and the analogues thereof by using a treatment solution to obtain the sample solution;
the sample liquid is used for laser excitation spectrum detection, and the use mode of the sample liquid comprises direct use, concentration use or use after dropping the sample liquid to a test piece and removing a solvent.
The invention relates to a laser excitation spectrum detection pretreatment method for black powder and analogues thereof.
The invention carries out pretreatment aiming at the black powder and the analogues thereof, overcomes the problems of inflammability and weak signals of the substances, has obvious progress, and has the following advantages compared with the prior art:
firstly, the method can not only overcome the problem of flammability of the black powder, but also greatly enhance the laser excitation spectrum signal of the black powder, and provide possibility for realizing safe and rapid detection of the black powder.
Secondly, the detection components of the method comprise one or more of potassium nitrate, ammonium nitrate, sodium nitrate, potassium perchlorate and potassium chlorate, and ammonium perchlorate, potassium chlorate, sodium perchlorate and ammonium chlorate, so that the application of the laser excitation spectrum technology in the detection of black powder and analogues thereof is greatly widened, and convenience is brought to the investigation and identification of dangerous objects.
Other characteristic features and advantages of the invention will become apparent from the following description of embodiments, which is to be read in connection with the accompanying drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the invention, in which like reference numerals are used to designate like elements, and the drawings in the following description are some, but not all embodiments of the invention, and will enable one of ordinary skill in the art to make and use the invention.
FIG. 1 is a flow chart of a method for pre-treating black powder and the like according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. It should be noted that the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without conflict.
In the embodiments 1 to 8 of the present invention, taking the pretreatment process of black powder as an example, 8g of black powder samples are equally divided into eight test samples, which are numbered as experiment groups 1 to 8, and each sample is 1 g.
Example 1
Treating black powder numbered as experimental group 1 with a treating fluid which is 20g of aqueous solution, adding the black powder into a beaker containing the treating fluid, heating and stirring for 2min at 50 ℃, fully dissolving, and filtering to remove precipitates when the solution is hot to obtain a sample solution 1 for later use.
Example 2
Preparing a treatment solution, adding 1g of hydrochloric acid solution with the concentration of 2% into 19g of water of the dispersion solution, acidifying the dispersion solution, and finally adding 0.002g of crown ether 18-crown-6; and treating the black powder numbered as experiment group 2 by using the prepared treatment solution, adding the black powder into a beaker filled with the treatment solution, stirring and oscillating for 5min, fully dissolving, centrifuging and removing precipitates to obtain a sample solution 2 for later use.
Examples 3 to 8
Examples 3 to 8 the preparation processes of examples 1 and 2 were referred to, and corresponding sample solutions 1 to 8 were prepared for future use. Wherein, in the mixing process of the treatment liquid and the black powder, one or more methods of stirring, shaking, ultrasonic treatment and heating can be selected, the slag removal process can be a filtering or centrifuging method, and the method can be selected by a person skilled in the art according to the actual situation. Generally, sonication, heating, and the like accelerate dissolution.
The mass of the treating fluid used in examples 1 to 8 was 20g, but the components and contents of the treating fluids were changed, and the specific examples are shown in table 1:
table 1 list of the components of the treatment fluids and their contents in the different examples
Figure GDA0002618362140000081
Figure GDA0002618362140000091
In table 1, the parenthesized values are the corresponding mass percentages of the components.
The sample liquid 1-8 is used for Raman spectrum detection, the sample liquid 2-8 can be directly detected except for the sample liquid 1 with high noise, the Raman spectrum signal is strong, accurate detection can be realized, and beneficial technical effects are achieved; the sample solution 1 is concentrated and then detected, so that accurate detection can be realized. And when the reinforcing agent is a mixture of two different crown ethers or derivatives thereof, the detection effect is best.
The whole pretreatment process of the embodiments 1 to 8 takes 5 to 10min, and it can be seen from the above embodiments that the pretreatment method provided by the invention not only can rapidly treat black powder and the like, but also overcomes the problems of flammability and weak signal of the black powder, and has significant progress, and compared with the prior art, the pretreatment method has the following advantages:
firstly, the method can not only overcome the problem of flammability of the black powder, but also greatly enhance the laser excitation spectrum signal of the black powder, and provide possibility for realizing safe and rapid detection of the black powder.
Secondly, the detection components of the method comprise one or more of potassium nitrate, ammonium nitrate, sodium nitrate, potassium perchlorate and potassium chlorate, ammonium perchlorate, sodium chlorate, sodium perchlorate and ammonium chlorate, so that the application of the laser excitation spectrum technology in the detection of black powder and the like is greatly widened, and convenience is brought to the investigation and identification work of dangerous objects.
The above-described aspects may be implemented individually or in various combinations, and such variations are within the scope of the present invention.
Finally, it should be noted that: in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only for illustrating the technical solutions of the present invention, and are not limited thereto. Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (8)

1. The pretreatment method of the black powder is characterized in that the black powder is treated by using a treatment fluid to obtain a sample fluid; the sample liquid is used for laser excitation spectrum detection, and the use mode of the sample liquid comprises direct use, concentration use or use after dropwise adding the sample liquid to a test piece and removing a solvent; wherein, the process of preparing the sample liquid comprises the following steps:
mixing: fully dissolving the black powder by using a treatment solution to prepare a mixed solution;
deslagging: removing the precipitate in the mixed solution to obtain a sample solution;
the processing liquid in the mixing step comprises a dispersion liquid and a reinforcing agent, wherein the reinforcing agent in the processing liquid accounts for 0.001-8% by mass, and the dispersion liquid is a polar solution containing water;
the reinforcing agent is a mixture of a reinforcing agent A and a reinforcing agent B, and the reinforcing agent A is selected from 18-crown-6; the reinforcing agent B is selected from 15-crown-5.
2. The pretreatment method for black powder according to claim 1, wherein the treatment solution further comprises an acidizing solution, the acidizing solution is one or more of a hydrochloric acid solution, a sulfuric acid solution and a nitric acid solution, and the acidizing solution in the treatment solution is 0-10% by mass.
3. The black powder pretreatment method according to claim 1, wherein the treatment fluid further comprises an acidizing fluid selected from the group consisting of: a hydrochloric acid solution with the volume concentration of 2-5%, wherein the addition amount is 4-6%; or 1-4% of sulfuric acid solution with volume concentration of 8-12%; or 4-6% of nitric acid solution with volume concentration of 4-9%.
4. The method of pretreating black powder according to claim 2, wherein said dispersion further comprises one or more of methanol, ethanol, acetonitrile and acetone.
5. The pretreatment method for black powder according to claim 1, wherein the dispersion is selected from the group consisting of water, a water/ethanol mixed solution in a volume ratio of 1:0.1 to 0.5, and a water/acetone mixed solution in a volume ratio of 1:0.2 to 0.8.
6. The black powder pretreatment method according to claim 1, wherein the mixing step comprises one or more of stirring, shaking, ultrasound, and heating, and the deslagging step comprises filtering or centrifuging.
7. The pretreatment method of black powder according to claim 1, further comprising preparing a treatment solution, wherein the pretreatment method comprises the following specific steps:
preparing a treatment liquid, wherein the treatment liquid comprises a dispersion liquid, an acidizing liquid and an intensifier, and the dispersion liquid is water, a water/ethanol mixed liquid or a water/acetone mixed liquid; adding an acidizing fluid for acidizing, wherein the acidizing fluid is a hydrochloric acid solution, a sulfuric acid solution or a nitric acid solution; finally adding a reinforcing agent, wherein the reinforcing agent is one or more of crown ether and crown ether derivatives;
preparing a sample solution, and treating the black powder by using a treatment solution to obtain the sample solution;
the sample liquid is used for laser excitation spectrum detection, and the use mode of the sample liquid comprises direct use, concentration use or use after dropping the sample liquid to a test piece and removing a solvent.
8. The pretreatment method for black powder according to claim 7, wherein in the step of preparing the treatment solution, the crown ether and the crown ether derivative comprise: 15-crown-5 and derivatives thereof, and 18-crown-6 and derivatives thereof, wherein the addition amount of the reinforcing agent is 0.001-8%.
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