CN101762562B - Method for measuring supersaturation degree of cyclotetramethylenetetranitramine process solution prepared by using CO2 gas solvent resistant method - Google Patents

Abstract

The invention relates to a method for measuring the supersaturation degree of a cyclotetramethylenetetranitramine process solution prepared by using a CO2 gas solvent resistant method, comprising the following steps of: vacuumizing; sampling; preparing a cyclotetramethylenetetranitramine acetonitrile sample solution; making a standard curve; and measuring the supersaturation degree of a cyclotetramethylenetetranitramine acetone solution. In the invention, samples are sampled by using a sampling pipe with both ends respectively connected with a high-pressure reaction kettle, the sampling pipe and the high-pressure reaction kettle are vacuumized so as to enable the solution to sufficiently flow in the sampling pipe and ensure the accurate sampling; meanwhile, sampled samples are measured by an ultraviolet spectrophotometer, thereby ensuring the accurate analysis and measurement and preventing the defects that the traditional weighing method can not accurately measure due to large errors and impurity influence and a colorimetric method has complicated steps; and in addition, the invention has easy operation and accurate test result.

Description

CO 2The gas anti-solvent method prepares the HMX-acetone soln method for measuring supersaturation degree in the HMX process

Technical field

The invention belongs to and utilize optical instrument, promptly utilize infrared light, visible light or ultraviolet light to test or the analysis of material technical field, be specifically related to use determination of ultra-violet CO ₂The gas anti-solvent method prepares the method for HMX process solution degree of supersaturation.

Background technology

CO ₂The gas anti-solvent method is a kind of new crystallization technique, is widely used in owing to the controllability of its operating conditions in the ultrafine dust preparation of energetic material.Through powder charge and use research proof to energetic material; Ultra-fine energetic material can significantly improve the powder charge performance; And the detonation property that effectively improves explosive is (high like explosion energy; Sensitivity is low, and the detonation wave propagation is more stable sooner etc.), therefore micronization, the super-refinement to energetic material has important use to be worth.CO ₂The gas anti-solvent method can be refined to submicron order even nanoscale with energetic material.Utilizing CO ₂The gas anti-solvent method prepares in the ultra-fine HMX particle process, and the key factor that granule size and size-grade distribution is played influence is the solution degree of supersaturation.Control solution degree of supersaturation just can realize the controllability of granule size and size-grade distribution, so it is most important to measure in the anti-dissolving agent process degree of supersaturation value.Not only simply but also accurately do not measure CO yet see as yet so far ₂The gas anti-solvent method prepares the report of HMX process solution degree of supersaturation.Traditional measurement degree of supersaturation method is a weight method, but CO ₂Gas anti-dissolving agent process organic solvent is to CO ₂The gas absorption amount is very big, can make the solution degree of supersaturation very big, and the particle amount of separating out is very big, causes in the solution contained solute amount seldom, and the solute that sampling obtains is bordering on trace, is difficult to measure with weight method.In addition, anti-dissolving agent process tends in the pipeline some impurity and brings the deposition still into, thereby impurity can be brought in the sampled sample in the sampling process, will certainly cause weighing inaccurate like this, produces very mistake.People such as Cai Jianguo (East China University of Science's doctorate paper; 69～70) method of utilizing nitroso-concentration in basic hydrolysis HMX, the colorimetric method for determining HMX is confirmed the concentration of HMX solution indirectly; And then obtain the solution degree of supersaturation; This method experimental procedure is various, and it is more loaded down with trivial details to operate, and causes very mistake easily.

Summary of the invention

Technical matters to be solved by this invention is to overcome the shortcoming of said determination method, and a kind of simple to operate, accurate test result CO is provided ₂The gas anti-solvent method prepares the HMX-acetone soln method for measuring supersaturation degree in the HMX process.

Solving the problems of the technologies described above the technical scheme that is adopted is that it comprises the steps:

1, vacuumizes

With vacuum pump autoclave and stopple coupon are vacuumized, the vacuum tightness that is evacuated to autoclave is 0.09MPa, in autoclave and stopple coupon, charges into CO ₂Gas, being charged to pressure is 0.5～1MPa, venting repeats to vacuumize twice again.

2, sampling

Getting HMX uses acetone by the HMX acetone soln of conventional method preparation mass concentration as 20mg/mL; Use syringe to draw the HMX acetone soln injection autoclave of mass concentration as 20mg/mL; Open attemperating unit; The reaction under high pressure temperature in the kettle is risen to 20～50 ℃, open CO ₂The valve of steel cylinder fills CO in high pressure syringe pump ₂Gas is opened high pressure syringe pump, compression CO ₂Gas makes in the gas storage tanks in advance that the swelling pressure reach 35MPa, opens the valve of autoclave, in autoclave, fills CO ₂Gas, the while high pressure syringe pump continues to replenish CO to autoclave with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 10～35MPa, precipitating 5 minutes; Open the feed liquor valve and the liquid valve at stopple coupon two ends successively, the solution that separates out particle in the autoclave is taken a sample, back out the nut at stopple coupon two ends; Take off stopple coupon, open the valve of knockout drum, carry out gas-liquid separation.

3, preparation HMX acetonitrile sample solution

The solution of getting in step 2 stopple coupon is changed in the beaker, be heated to 50～80 ℃, solvent evaporated acetone; Be cooled to room temperature, add acetonitrile, the dissolving HMX; Lysate is transferred in the volumetric flask, and with acetonitrile rinse beaker 2～3 times, rinse liquid is transferred in the volumetric flask in the lump; Add acetonitrile and be settled to scale mark, be mixed with HMX acetonitrile sample solution.

4, production standard curve

Getting HMX use acetonitrile is the HMX acetonitrile standard solution of 100 μ g/mL by conventional method preparation mass concentration; Use transfer pipet measures 1,2,3,4,5,6,7 respectively, the 8mL mass concentration is 100 μ g/mL HMX acetonitrile standard solution to place the volumetric flask of 8 50mL; Add acetonitrile and be settled to scale mark; Be made into mass concentration and be respectively the HMX acetonitrile standard solution of 2,4,6,8,10,12,14,16 μ g/mL; In maximum absorption wavelength 226nm place, is ordinate with the absorbance that records with ultraviolet spectrophotometer, and the mass concentration of corresponding HMX acetonitrile standard solution is a horizontal ordinate; Drawing standard curve, typical curve equation are formula (1):

A＝0.06428C-0.00534 (1)

A is the absorbance of HMX acetonitrile standard solution in the formula, and C is the mass concentration of HMX acetonitrile standard solution, and coefficient R is 0.9998.

5, measure HMX acetone soln degree of supersaturation

The HMX acetonitrile sample solution of step 3 preparation is measured solution absorbency with ultraviolet spectrophotometer in maximum absorption wavelength 226nm place; According to the mass concentration of typical curve equation (1) calculating HMX acetonitrile sample solution, by formula the equilibrium concentration of HMX acetone soln is calculated in (2):

$C_e=\frac{{\mathrm{<figure-callout\; id="1"\; label="C"\; filenames="H2009102546211E00011.png"\; state="\{\{state\}\}">C</figure-callout>}}_1\&CenterDot;{\mathrm{<figure-callout\; id="1"\; label="V"\; filenames="H2009102546211E00011.png"\; state="\{\{state\}\}">V</figure-callout>}}_1\&CenterDot;({\mathrm{<figure-callout\; id="2"\; label="V"\; filenames="H2009102546211E00012.png"\; state="\{\{state\}\}">V</figure-callout>}}_2+V_3)}{{\mathrm{<figure-callout\; id="2"\; label="V"\; filenames="H2009102546211E00012.png"\; state="\{\{state\}\}">V</figure-callout>}}_2{\&CenterDot;V}_4}---\left(2\right)$

C in the formula _eBe the equilibrium concentration of HMX acetone soln, C ₁Be the mass concentration of HMX acetonitrile sample solution, V ₁Be the volume of volumetric flask in the step 3, V ₂Be the volume of stopple coupon, V ₃Be the volume of autoclave, V ₄Volume for the HMX acetone soln that adds during syringe sampling in the step 2, calculate HMX acetone soln degree of supersaturation according to formula (3):

$S=\frac{C_0}{C_e}---\left(3\right)$

S is a HMX acetone soln degree of supersaturation in the formula, C ₀Mass concentration 20mg/mL for the HMX acetone soln that adds during syringe sampling in the step (2).

The present invention adopts the stopple coupon sampling, and the stopple coupon two ends are connected on the autoclave respectively, and stopple coupon and autoclave are vacuumized processing, so that solution is fully mobile in stopple coupon, guarantees that sampling accurately.Simultaneously institute's collected specimens is measured with ultraviolet spectrophotometer; Guarantee the accurate of analysis to measure; Avoided that traditional weight method error is big, impurity effect and can not accurately measuring, the shortcoming that the colourimetry step is lengthy and tedious has simple to operate, accurate test result advantage.

Description of drawings

Fig. 1 uses CO ₂The gas anti-solvent method prepares the apparatus structure synoptic diagram of HMX ultrafine dust.

Fig. 2 is that ultraviolet spectrophotometer records variable concentrations HMX-acetonitrile solution typical curve at wavelength 226nm place.

Embodiment

To further explain of the present invention, but the invention is not restricted to these embodiment below in conjunction with accompanying drawing and embodiment.

Embodiment 1

1, vacuumizes

Use vacuum pump 1 that the autoclave 4 of volume as 60mL vacuumized with the stopple coupon 5 of volume as 19mL, the vacuum tightness that is evacuated to autoclave 4 is 0.09MPa, in autoclave 4 and stopple coupon 5, charges into CO ₂Gas, being charged to pressure is 0.5～1MPa, venting repeats to vacuumize twice again.

2, sampling

Getting HMX uses acetone by the HMX acetone soln of conventional method preparation mass concentration as 20mg/mL; Use syringe 3 to draw the HMX acetone soln 10mL injection autoclave 4 of mass concentration as 20mg/mL; Open attemperating unit 7; Temperature in the autoclave 4 is risen to 20 ℃, open CO ₂The valve of steel cylinder 9 fills CO in high pressure syringe pump 8 ₂Gas is opened high pressure syringe pump 8, compression CO ₂Gas makes in the gas storage tanks 2 in advance that the swelling pressure reach 35MPa, opens the valve of autoclave 4, in autoclave 4, fills CO ₂Gas, while high pressure syringe pump 8 continues to replenish CO to autoclave 4 with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 10MPa, precipitating 5 minutes; Open the feed liquor valve and the liquid valve at stopple coupon 5 two ends successively, the solution that separates out particle in the autoclave 4 is taken a sample, back out the nut at stopple coupon 5 two ends; Take off stopple coupon 5, open the valve of knockout drum 6, carry out gas-liquid separation.

3, preparation HMX acetonitrile sample solution

The solution of getting in step 2 stopple coupon 5 is changed in the 50mL beaker, be heated to 50～80 ℃, solvent evaporated acetone; Be cooled to room temperature, add 1～2mL acetonitrile, the dissolving HMX; Lysate is transferred in the 250mL volumetric flask, and with acetonitrile rinse beaker 2～3 times, rinse liquid is transferred in the volumetric flask in the lump; Add acetonitrile and be settled to scale mark, be mixed with HMX acetonitrile sample solution.

4, production standard curve

Using HMX and acetonitrile is the HMX acetonitrile standard solution of 100 μ g/mL by conventional method preparation mass concentration; Use transfer pipet measures 1,2,3,4,5,6,7 respectively, the 8mL mass concentration is 100 μ g/mL HMX acetonitrile standard solution to place the volumetric flask of 8 50mL; Add acetonitrile and be settled to scale mark; Be made into mass concentration and be respectively the HMX acetonitrile standard solution of 2,4,6,8,10,12,14,16 μ g/mL; In maximum absorption wavelength 226nm place, is ordinate with the absorbance that records with ultraviolet spectrophotometer, and the mass concentration of corresponding HMX acetonitrile standard solution is a horizontal ordinate; Drawing standard curve, typical curve equation are formula (1):

A＝0.06428C-0.00534 (1)

A is the absorbance of HMX acetonitrile standard solution in the formula, and C is the mass concentration of HMX acetonitrile standard solution, and coefficient R is 0.9998, and resulting typical curve is seen Fig. 2.

5, measure HMX acetone soln degree of supersaturation

With the HMX acetonitrile sample solution of step 3 preparation with ultraviolet spectrophotometer in maximum absorption wavelength 226nm place; Recording solution absorbency is 0.437; Calculate the mass concentration of HMX acetonitrile sample solution according to typical curve equation (1); Through calculating, the mass concentration of HMX acetonitrile sample solution is 6.88 μ g/mL, and by formula the equilibrium concentration of HMX acetone soln is calculated in (2):

$C_e=\frac{{\mathrm{<figure-callout\; id="1"\; label="C"\; filenames="H2009102546211E00011.png"\; state="\{\{state\}\}">C</figure-callout>}}_1\&CenterDot;{\mathrm{<figure-callout\; id="1"\; label="V"\; filenames="H2009102546211E00011.png"\; state="\{\{state\}\}">V</figure-callout>}}_1\&CenterDot;({\mathrm{<figure-callout\; id="2"\; label="V"\; filenames="H2009102546211E00012.png"\; state="\{\{state\}\}">V</figure-callout>}}_2+V_3)}{{\mathrm{<figure-callout\; id="2"\; label="V"\; filenames="H2009102546211E00012.png"\; state="\{\{state\}\}">V</figure-callout>}}_2{\&CenterDot;V}_4}---\left(2\right)$

C in the formula ₁Be the mass concentration 6.88 μ g/mL of HMX acetonitrile sample solution, V ₁Be the volume 250mL of volumetric flask in the step 3, V ₂Be the volume 19mL of stopple coupon 5, V ₃Be the volume 60mL of autoclave 4, V ₄Volume 10mL for the HMX acetone soln that adds during syringe sampling in the step 2.Through calculating the equilibrium concentration C of HMX acetone soln _eBe 715.16 μ g/mL, calculate HMX acetone soln degree of supersaturation according to formula (3):

$S=\frac{C_0}{C_e}---\left(3\right)$

S is a HMX acetone soln degree of supersaturation in the formula, C ₀Be the mass concentration 20mg/mL of the HMX acetone soln that adds during syringe sampling in the step 2, through calculating, HMX acetone soln degree of supersaturation S is 27.97.

Embodiment 2

In present embodiment sampling procedure 2, high pressure syringe pump 8 continues to replenish CO to autoclave 4 with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 15MPa, other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, and the absorbance that records HMX acetonitrile sample solution is 0.430, and through calculating, the mass concentration of HMX acetonitrile sample solution is 6.77 μ g/mL, the equilibrium concentration C of HMX acetone soln _eBe 703.72 μ g/mL, HMX acetone soln degree of supersaturation S is 28.42.

Embodiment 3

In present embodiment sampling procedure 2, high pressure syringe pump 8 continues to replenish CO to autoclave 4 with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 20MPa, other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, and the absorbance that records HMX acetonitrile sample solution is 0.409, and through calculating, the mass concentration of HMX acetonitrile sample solution is 6.45 μ g/mL, the equilibrium concentration C of HMX acetone soln _eBe 670.46 μ g/mL, HMX acetone soln degree of supersaturation S is 29.83.

Embodiment 4

In present embodiment sampling procedure 2, high pressure syringe pump 8 continues to replenish CO to autoclave 4 with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 25MPa, other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, and the absorbance that records HMX acetonitrile sample solution is 0.229, and through calculating, the mass concentration of HMX acetonitrile sample solution is 3.65 μ g/mL, the equilibrium concentration C of HMX acetone soln _eBe 379.41 μ g/mL, HMX acetone soln degree of supersaturation S is 52.71.

Embodiment 5

In present embodiment sampling procedure 2, high pressure syringe pump 8 continues to replenish CO to autoclave 4 with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 30MPa, other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, and the absorbance that records HMX acetonitrile sample solution is 0.150, and through calculating, the mass concentration of HMX acetonitrile sample solution is 2.42 μ g/mL, the equilibrium concentration C of HMX acetone soln _eBe 251.55 μ g/mL, HMX acetone soln degree of supersaturation S is 79.51.

Embodiment 6

In present embodiment sampling procedure 2, high pressure syringe pump 8 continues to replenish CO to autoclave 4 with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 35MPa, other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, and the absorbance that records HMX acetonitrile sample solution is 0.149, and through calculating, the mass concentration of HMX acetonitrile sample solution is 2.40 μ g/mL, the equilibrium concentration C of HMX acetone soln _eBe 249.47 μ g/mL, HMX acetone soln degree of supersaturation S is 80.17.

Embodiment 7

In present embodiment sampling procedure 2, open attemperating unit 7, temperature in the autoclave 4 is risen to 30 ℃, high pressure syringe pump 8 continues to replenish CO to autoclave 4 with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 10MPa, other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, and the absorbance that records HMX acetonitrile sample solution is 0.937, and through calculating, the mass concentration of HMX acetonitrile sample solution is 14.66 μ g/mL, the equilibrium concentration C of HMX acetone soln _eBe 1523.87 μ g/mL, HMX acetone soln degree of supersaturation S is 13.12.

Embodiment 8

In present embodiment sampling procedure 2, open attemperating unit 7, temperature in the autoclave 4 is risen to 30 ℃, high pressure syringe pump 8 continues to replenish CO to autoclave 4 with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 35MPa, other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, and the absorbance that records HMX acetonitrile sample solution is 0.623, and through calculating, the mass concentration of HMX acetonitrile sample solution is 9.78 μ g/mL, the equilibrium concentration C of HMX acetone soln _eBe 1016.61 μ g/mL, HMX acetone soln degree of supersaturation S is 19.67.

Embodiment 9

In present embodiment sampling procedure 2, open attemperating unit 7, temperature in the autoclave 4 is risen to 40 ℃, high pressure syringe pump 8 continues to replenish CO to autoclave 4 with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 10MPa, other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, and the absorbance that records HMX acetonitrile sample solution is 0.335, and through calculating, the mass concentration of HMX acetonitrile sample solution is 5.29 μ g/mL, the equilibrium concentration C of HMX acetone soln _eBe 549.88 μ g/mL, HMX acetone soln degree of supersaturation S is 36.37.

Embodiment 10

In present embodiment sampling procedure 2, open attemperating unit 7, temperature in the autoclave 4 is risen to 40 ℃, high pressure syringe pump 8 continues to replenish CO to autoclave 4 with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 35MPa, other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, and the absorbance that records HMX acetonitrile sample solution is 0.359, and through calculating, the mass concentration of HMX acetonitrile sample solution is 5.67 μ g/mL, the equilibrium concentration C of HMX acetone soln _eBe 589.38 μ g/mL, HMX acetone soln degree of supersaturation S is 33.93.

Embodiment 11

In present embodiment sampling procedure 2, open attemperating unit 7, temperature in the autoclave 4 is risen to 50 ℃, high pressure syringe pump 8 continues to replenish CO to autoclave 4 with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 10MPa, other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, and the absorbance that records HMX acetonitrile sample solution is 0.384, and through calculating, the mass concentration of HMX acetonitrile sample solution is 6.06 μ g/mL, the equilibrium concentration C of HMX acetone soln _eBe 629.92 μ g/mL, HMX acetone soln degree of supersaturation S is 31.75.

Embodiment 12

In present embodiment sampling procedure 2, open attemperating unit 7, temperature in the autoclave 4 is risen to 50 ℃, high pressure syringe pump 8 continues to replenish CO to autoclave 4 with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 35MPa, other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, and the absorbance that records HMX acetonitrile sample solution is 0.399, and through calculating, the mass concentration of HMX acetonitrile sample solution is 6.29 μ g/mL, the equilibrium concentration C of HMX acetone soln _eBe 653.83 μ g/mL, HMX acetone soln degree of supersaturation S is 30.59.

Claims (1)

1. CO ₂The gas anti-solvent method prepares the HMX-acetone soln method for measuring supersaturation degree in the HMX process, it is characterized in that it comprises the steps:

(1) vacuumizes

With vacuum pump (1) autoclave (4) and stopple coupon (5) are vacuumized, the vacuum tightness that is evacuated to autoclave (4) is 0.09MPa, in autoclave (4) and stopple coupon (5), charges into CO ₂Gas, being charged to pressure is 0.5～1MPa, venting repeats to vacuumize twice again;

(2) sampling

Getting HMX uses acetone by the HMX-acetone soln of conventional method preparation mass concentration as 20mg/mL; Draw the HMX that mass concentration is 20mg/mL-acetone soln with syringe (3) and inject autoclave (4); Open attemperating unit (7); The interior temperature of autoclave (4) is risen to 20～50 ℃, open CO ₂The valve of steel cylinder (9) fills CO in high pressure syringe pump (8) ₂Gas is opened high pressure syringe pump (8), compression CO ₂Gas makes in the gas storage tanks (2) in advance that the swelling pressure reach 35MPa, opens the valve of autoclave (4), in autoclave (4), fills CO ₂Gas, while high pressure syringe pump (8) continues to replenish CO to autoclave (4) with 30mL/ minute air inlet speed ₂Gas, being supplemented to pressure is 10～35MPa, precipitating 5 minutes; Open the feed liquor valve and the liquid valve at stopple coupon (5) two ends successively; Solution to separating out particle in the autoclave (4) is taken a sample, and backs out the nut at stopple coupon (5) two ends, takes off stopple coupon (5); Open the valve of knockout drum (6), carry out gas-liquid separation;

(3) preparation HMX acetonitrile sample solution

The solution of getting in step (2) stopple coupon (5) is changed in the beaker, be heated to 50～80 ℃, solvent evaporated acetone; Be cooled to room temperature, add acetonitrile, the dissolving HMX; Lysate is transferred in the volumetric flask, and with acetonitrile rinse beaker 2～3 times, rinse liquid is transferred in the volumetric flask in the lump; Add acetonitrile and be settled to scale mark, be mixed with HMX acetonitrile sample solution;

(4) production standard curve

Using HMX and acetonitrile is the HMX acetonitrile standard solution of 100 μ g/mL by conventional method preparation mass concentration; Use transfer pipet measures 1,2,3,4,5,6,7 respectively, the 8mL mass concentration is 100 μ g/mL HMX acetonitrile standard solution to place the volumetric flask of 8 50mL; Add acetonitrile and be settled to scale mark; Be made into mass concentration and be respectively the HMX acetonitrile standard solution of 2,4,6,8,10,12,14,16 μ g/mL; In maximum absorption wavelength 226nm place, is ordinate with the absorbance that records with ultraviolet spectrophotometer, and the mass concentration of corresponding HMX acetonitrile standard solution is a horizontal ordinate; Drawing standard curve, typical curve equation are formula (1):

A＝0.06428C-0.00534 (1)

A is the absorbance of HMX acetonitrile standard solution in the formula, and C is the mass concentration of HMX acetonitrile standard solution, and coefficient R is 0.9998;

(5) measure HMX acetone soln degree of supersaturation

The HMX acetonitrile sample solution of step (3) preparation is measured solution absorbency with ultraviolet spectrophotometer in maximum absorption wavelength 226nm place; According to the mass concentration of typical curve equation (1) calculating HMX acetonitrile sample solution, by formula the equilibrium concentration of HMX acetone soln is calculated in (2):

C in the formula _eBe the equilibrium concentration of HMX acetone soln, C ₁Be the mass concentration of HMX acetonitrile sample solution, V ₁Be the volume of volumetric flask in the step (3), V ₂Be the volume of stopple coupon (5), V ₃Be the volume of autoclave (4), V ₄Volume for the HMX acetone soln that adds during syringe (3) sample introduction in the step (2), calculate HMX acetone soln degree of supersaturation according to formula (3):

S is a HMX acetone soln degree of supersaturation in the formula, C ₀Mass concentration 20mg/mL for the HMX acetone soln that adds during syringe (3) sample introduction in the step (2).

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