CN112505022A - Method for measuring nitride in gunpowder emission ablation product - Google Patents
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- 150000004767 nitrides Chemical class 0.000 title claims abstract description 36
- 238000002679 ablation Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000003721 gunpowder Substances 0.000 title claims abstract description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 40
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000012265 solid product Substances 0.000 claims abstract description 35
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 32
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims abstract description 24
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000000047 product Substances 0.000 claims abstract description 21
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims abstract description 17
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 10
- 238000010992 reflux Methods 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000009833 condensation Methods 0.000 claims abstract description 7
- 230000005494 condensation Effects 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 238000000967 suction filtration Methods 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 4
- 238000007431 microscopic evaluation Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 238000005406 washing Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000011088 calibration curve Methods 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003380 propellant Substances 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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Abstract
The invention discloses a method for measuring nitride in gunpowder launching ablation products, which comprises the following steps: mixing a sample to be detected with bromine and methyl acetate, carrying out condensation reflux reaction for 2-4 h at 60-70 ℃, cooling, carrying out reduced pressure suction filtration to obtain nitride residues, and cleaning and drying the residues to obtain a solid product A; mixing the solid product A with nitric acid, hydrofluoric acid and perchloric acid to react so as to completely dissolve the solid, and heating to evaporate the solvent to obtain a solid product B; mixing the solid product B with acid, heating at 50-100 ℃ for 10-30 min, and cooling to obtain a solution to be detected; and detecting the solution to be detected by using a plasma emission spectrometer to obtain the content of the nitride. The method realizes the separation and analysis of the nitride in the emission ablation product, overcomes the limitation that the existing microscopic analysis method is limited by knowledge and experience of researchers, and can accurately and quantitatively analyze the attribute of the nitride in the ablation product. The method is simple and convenient to operate, small in artificial influence factor and high in result accuracy.
Description
Technical Field
The invention belongs to the technical field of material analysis, and particularly relates to a method for measuring nitride in gunpowder emission ablation products.
Background
The barrel weapon is used for being matched with gunpowder gas, and endows the projectile with certain initial speed and rotation speed for ensuring stable flight of the projectile. In recent years, with the development of high initial speed, high firing speed and long-range barrel weapons, the barrel is also subjected to more and more serious thermophysical chemical action of propellant gas, scouring of high-speed flowing gas and abrasion action of a projectile, and the problem of barrel ablatability is increasingly prominent.
Under high temperature and high pressure, propellant gas and barrel material react chemically to produce hard and brittle oxide, carbide, nitride, etc. with low melting point, and the surface thin layer containing these newly produced compounds is easy to crack, scour by airflow or rub by bullet belt, resulting in high ablation. In the ablation product, oxides and carbides are considered to be the main existing forms, so that the corresponding detection is easier to realize. And the nitride is often included in other ablation products and is not easy to be directly observed. At present, no specific method for quantitative analysis of nitride in the emission ablation product is found, which seriously restricts the deep development of the emission ablation research.
Disclosure of Invention
Aiming at the technical requirements, the invention provides a method for measuring nitride in the gunpowder emission ablation product, and the problem of quantitative analysis of the nitride in the emission ablation product is solved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for measuring nitride in gunpowder emission ablation products comprises the following steps:
step 1, mixing a sample to be detected with bromine and methyl acetate, carrying out condensation reflux reaction for 2-4 h at the temperature of 60-70 ℃, cooling, carrying out reduced pressure suction filtration to obtain nitride residues, and cleaning and drying the residues to obtain a solid product A; the mass of the sample to be detected and the volume ratio of bromine are within the range of 1: 3-1: 4, and the volume ratio of bromine and methyl acetate is within the range of 1: 5-1: 4;
step 2, mixing the solid product A obtained in the step 1 with nitric acid, hydrofluoric acid and perchloric acid to react so as to completely dissolve the solid, and heating to evaporate the solvent to obtain a solid product B; the mass ratio of the solid product A to the total substances added with nitric acid, hydrofluoric acid and perchloric acid is 1g: 8-20 mol;
step 3, mixing the solid product B with acid, heating for 10-30 min at 50-100 ℃, and cooling to obtain a solution to be detected;
and 4, detecting the solution to be detected by using a plasma emission spectrometer to obtain the content of the nitride.
Preferably, in the step 1, a sample to be detected is mixed with bromine, methyl acetate is added into the mixed system for multiple times in the reaction process, and the interval time of each time is 15-20 min.
Preferably, in the step 2, the solid product a is firstly mixed with nitric acid and hydrofluoric acid, and after reaction for 10-30 min, perchloric acid is added for reaction until the solid is completely dissolved.
Preferably, in the step 2, the nitric acid, the hydrofluoric acid and the perchloric acid are mixed according to a molar ratio of 1:1.5: 0.8.
Preferably, in the step 2, the heating and drying temperature is 150-200 ℃, and the time is 0.5-2 h.
Preferably, the acid in the step 3 is a mixed acid of deionized water, nitric acid and hydrochloric acid, wherein the molar ratio of the deionized water to the nitric acid is 1: 150-1: 170, and the molar ratio of the nitric acid to the hydrochloric acid is 1: 0.8.
Compared with the prior art, the invention has the beneficial effects that:
the method realizes the separation and analysis of the nitride in the emission ablation product, overcomes the limitation that the existing microscopic analysis method is limited by knowledge and experience of researchers, and can accurately and quantitatively analyze the attribute of the nitride in the ablation product. The method is simple and convenient to operate, small in artificial influence factor and high in result accuracy.
Drawings
FIG. 1 is a calibration curve relating intensity to concentration obtained in example 4.
FIG. 2 is a surface view of solid product A from example 1.
Detailed Description
The invention discloses a method for measuring nitride in gunpowder emission ablation products, which comprises the steps of separating the nitride in an emission ablation sample, and measuring the content by using a plasma emission spectrometer and other equipment. The method specifically comprises the following steps:
step 1, mixing a sample to be detected with bromine and methyl acetate, carrying out condensation reflux reaction for 2-4 h at 60-70 ℃ to completely dissolve matrix metal of the sample to be detected, cooling, carrying out reduced pressure suction filtration to obtain nitride residues, and cleaning and drying the residues to obtain a solid product A.
The methyl acetate is preferably added in the following manner: firstly, a sample to be detected and bromine are mixed in a reaction vessel, the specific reaction vessel is a condensation reflux device, and then a small amount of methyl acetate is introduced, preferably, the amount of methyl acetate added for the first time is mixed according to the ratio of the mass of the sample to be detected to the volume of the methyl acetate of 1: 2.5; and then heating the system to 60-70 ℃ for condensation reflux reaction for 2-4 h, and adding methyl acetate into the mixed system for multiple times in the reaction process, wherein the interval time of each time is 15-20 min.
In the invention, the ratio of the mass of the sample to be detected to the volume of bromine is 1: 3-1: 4, and the total volume ratio of bromine to methyl acetate is 1: 5-1: 4.
Step 2, mixing the solid product A obtained in the step 1 with nitric acid, hydrofluoric acid and perchloric acid for reaction to completely dissolve the solid, specifically reacting until no solid can be seen in the mixed solution; then heating to evaporate the solvent to obtain a solid product B. Wherein the mass ratio of the solid product A to the total mass of the added nitric acid, hydrofluoric acid and perchloric acid is 1g: 8-20 mol. More preferably, the nitric acid, the hydrofluoric acid and the perchloric acid are mixed in a molar ratio of 1:1.5: 0.8.
The addition method of the nitric acid, the hydrofluoric acid and the perchloric acid in the invention is preferably as follows: firstly, mixing a solid product A with nitric acid and hydrofluoric acid, reacting for 10-30 min, and then adding perchloric acid to react until the solid is completely dissolved.
The temperature for heating and evaporating to dryness in the invention is preferably 150-200 ℃, and the time is 0.5-2 h.
And 3, mixing the solid product B with acid, heating at 50-100 ℃ for 10-30 min, and cooling to obtain a solution to be detected. In the step, deionized water and a mixed acid of nitric acid and hydrochloric acid are preferably selected as the acid, wherein the molar ratio of the deionized water to the nitric acid is 1: 150-1: 170, and the molar ratio of the nitric acid to the hydrochloric acid is 1: 0.8.
And 4, detecting the solution to be detected by using a plasma emission spectrometer to obtain the content of the metal elements in the nitride.
The following embodiments of the present invention are provided, and it should be noted that the present invention is not limited to the following embodiments, and all equivalent changes based on the technical solutions of the present invention are within the protection scope of the present invention.
Bromine, methyl acetate, nitric acid, hydrofluoric acid, perchloric acid, hydrochloric acid, which are used in the following examples of the present invention, are commercially available.
Example 1
Step 1, weighing 0.1g of sample to be detected, placing the sample to be detected in a reaction bottle of an ester-halogen extractor, adding 0.3mL of bromine, connecting a condensing device and then connecting condensed water. Then 0.25mL of methyl acetate was added via the condenser. Methyl acetate was then added in five additional portions every 15min, each 0.25 mL. Condensing and refluxing at the heating temperature of 70 ℃, and reacting for 2 hours until the matrix metal is completely dissolved. Cooling, vacuum filtering to obtain nitride residue, washing the residue with methyl acetate for 4 times, washing with water for 2 times, and vacuum drying at 50 deg.C for 48 hr to obtain solid product A. As shown in fig. 2, it was confirmed by surface scanning analysis that a contained a large amount of nitrogen and the metal element was mainly iron.
Step 2, transferring the obtained solid product A to a polytetrafluoroethylene beaker, adding 4mL of nitric acid with the concentration of 15.0mol/L and 4mL of hydrofluoric acid with the concentration of 22.5mol/L, adding 4mL of perchloric acid after the reaction is stopped, and placing the mixture on an electric heating furnace for heating and drying to dryness, wherein the heating and drying temperature of the embodiment is 150-200 ℃, so as to obtain a solid product B;
and 3, cooling the solid product B, adding 8mL of water, 4mL of nitric acid with the concentration of 15.0mol/L and 4mL of hydrochloric acid with the concentration of 12mol/L, and heating for 10 min. Cooling, then using water to fix and hold in a 100mL volumetric flask, and mixing uniformly to obtain the solution to be measured 1 #.
Example 2
Step 1, weighing 0.3g of a sample to be detected, placing the sample to be detected in a reaction bottle of an ester-halogen extractor, adding 1mL of bromine, connecting a condensing device, and then connecting condensed water. Then 0.75mL of methyl acetate was added via the condenser. Methyl acetate was then added in five additional portions, 0.75mL each, every 18 min. Condensing and refluxing the mixture at the heating temperature of 60 ℃ and reacting for 3 hours. Cooling, vacuum filtering to obtain nitride residue, washing the residue with methyl acetate for 4 times, washing with water for 2 times, and vacuum drying at 50 deg.C for 48 hr to obtain solid product A.
Step 2, transferring the obtained solid product A to a polytetrafluoroethylene beaker, adding 6mL of nitric acid and 6mL of hydrofluoric acid, adding 6mL of perchloric acid after the reaction is stopped, placing the mixture on an electric heating furnace, heating and evaporating to dryness to obtain a solid product B;
and 3, cooling the solid product B, adding 10mL of water, 6mL of nitric acid and 6mL of hydrochloric acid, and heating for 10min to dissolve salts. Cooling, then using water to fix and hold in a 100mL volumetric flask, and mixing uniformly to obtain the solution 2# to be measured. The concentrations of nitric acid, hydrofluoric acid, perchloric acid and hydrochloric acid used in this example were the same as in example 1.
Example 3
0.5g of a sample to be measured is weighed, placed in a reaction flask of an ester-halogen extractor, added with 1.5mL of bromine, connected with a condensing device and then communicated with condensed water. Then 1.25mL of methyl acetate was added via the condenser. Methyl acetate was then added in five additional portions, 1.25mL each, every 20 min. And carrying out condensation reflux at the heating temperature of 65 ℃, and reacting for 4 hours until the matrix metal is completely dissolved. Cooling, vacuum filtering to obtain nitride residue, washing the residue with methyl acetate for 4 times, washing with water for 2 times, and vacuum drying at 50 deg.C for 48 hr to obtain solid product A.
Step 2, transferring the obtained solid product to a polytetrafluoroethylene beaker, adding 8mL of nitric acid and 8mL of hydrofluoric acid, adding 8mL of perchloric acid after the reaction is stopped, placing the mixture on an electric heating furnace, heating and evaporating to dryness to obtain a solid product B;
and 3, cooling the solid product B, adding 12mL of water, 8mL of nitric acid and 8mL of hydrochloric acid, and heating for 10min to dissolve salts. Cooling, then putting the solution into a 100mL volumetric flask with water, and mixing uniformly to obtain the solution to be measured No. 3. The concentrations of nitric acid, hydrofluoric acid, perchloric acid and hydrochloric acid used in this example were the same as in example 1.
Example 4
Preparing 1 mug/mL iron standard solution for standby. 0, 2.0mL, 4.0mL, 6.0mL and 8.0mL are respectively transferred and put into 5 100mL volumetric flasks, 0.5mL of hydrochloric acid is added into each flask, diluted to the scale and mixed evenly. The plasma emission spectrometer was used for detection to obtain a calibration curve relating intensity to concentration, as shown in fig. 1. And fitting the calibration curve to obtain a linear regression equation: y is 17748x +17.5 and the linear correlation coefficient is R2＝0.9999。
The three solutions 1#, 2#, and 3# to be tested in examples 1-3 were tested by the plasma emission spectrometer, and each sample was tested five times, and the results are shown in table 1 below, where the average value in table 1 refers to the percentage content of iron element in the solution to be tested.
TABLE 1 test results for three test solutions of examples 1-3
It can be seen that the relative standard deviation of the test results of the above examples is low, the method of the present invention has high precision, and the properties of the nitride in the ablation product can be quantitatively analyzed.
It should be noted that, in this embodiment, only the content of the iron element in the nitride is tested, so as to verify the accuracy of the measuring method of the present invention, and when the content of other elements in the nitride is measured, corresponding standard solutions are required to be configured, and the measuring method is the same as that of the iron element.
Claims (6)
1. A method for measuring nitride in gunpowder emission ablation products is characterized by comprising the following steps:
step 1, mixing a sample to be detected with bromine and methyl acetate, carrying out condensation reflux reaction for 2-4 h at the temperature of 60-70 ℃, cooling, carrying out reduced pressure suction filtration to obtain nitride residues, and cleaning and drying the residues to obtain a solid product A; the mass of the sample to be detected and the volume ratio of bromine are within the range of 1: 3-1: 4, and the volume ratio of bromine and methyl acetate is within the range of 1: 5-1: 4;
step 2, mixing the solid product A obtained in the step 1 with nitric acid, hydrofluoric acid and perchloric acid to react so as to completely dissolve the solid, and heating to evaporate the solvent to obtain a solid product B;
the mass ratio of the solid product A to the total substances added with nitric acid, hydrofluoric acid and perchloric acid is 1g: 8-20 mol;
step 3, mixing the solid product B with acid, heating for 10-30 min at 50-100 ℃, and cooling to obtain a solution to be detected;
and 4, detecting the solution to be detected by using a plasma emission spectrometer to obtain the content of the metal elements in the nitride.
2. The method for measuring the nitrides in the gunpowder launching ablation products as claimed in claim 1, wherein in the step 1, the sample to be measured is firstly mixed with bromine, methyl acetate is added into the mixed system for multiple times in the reaction process, and the interval time of each time is 15-20 min.
3. The method for measuring the nitrides in the gunpowder emission ablation product as claimed in claim 1, wherein in the step 2, firstly, the solid product A is mixed with nitric acid and hydrofluoric acid, and after the reaction for 10-30 min, perchloric acid is added for reaction until the solid is completely dissolved.
4. The method for measuring nitride in gunpowder firing ablation product according to claim 1 or 3, wherein the nitric acid, hydrofluoric acid and perchloric acid are mixed in a molar ratio of 1:1.5:0.8 in the step 2.
5. The method for measuring the nitrides in the gunpowder emission ablation products as claimed in claim 1, wherein in the step 2, the heating and evaporating temperature is 150-200 ℃ and the time is 0.5-2 h.
6. The method for measuring nitrides in powder emission ablation products according to claim 1, wherein the acid in the step 3 is a mixed acid of deionized water, nitric acid and hydrochloric acid, wherein the molar ratio of the deionized water to the nitric acid is 1: 150-1: 170, and the molar ratio of the nitric acid to the hydrochloric acid is 1: 0.8.
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