CN112683841A - Preparation method of ammonium perchlorate standard samples with different water contents - Google Patents
Preparation method of ammonium perchlorate standard samples with different water contents Download PDFInfo
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Abstract
The invention provides a preparation method of ammonium perchlorate standard samples with different water contents, belonging to the technical field of standard sample preparation. According to the method, the relationship between the porosity and the water content of the ammonium perchlorate powder is fully considered, the ammonium perchlorate standard sample is prepared in different modes according to different water contents, and water with different contents can be uniformly distributed in the pores of the ammonium perchlorate powder. Meanwhile, the influence of the standing time on the water diffusion is fully considered, the uniform diffusion of water among the pores of the ammonium perchlorate powder can be ensured by limiting the standing time in the preparation process of the ammonium perchlorate standard sample with different water contents, and the water in the obtained ammonium perchlorate standard sample is uniformly distributed.
Description
Technical Field
The invention relates to the technical field of standard sample preparation, in particular to a preparation method of ammonium perchlorate standard samples with different water contents.
Background
Ammonium Perchlorate (AP) has the advantages of high effective oxygen content, no heavy metal ions, good process performance, higher thermal stability, chemical stability and the like, and is widely used as an oxidant for energetic materials such as pyrotechnic compositions, blasting explosives, solid rocket propellants and the like. Research shows that moisture can adversely affect the combustion energy release, the combustion speed, the mechanical properties, the mechanical sensitivity and the like of the energetic material. Therefore, the moisture content of AP is regulated in GJB 617A-2003 ammonium perchlorate as a project and a technical index which are necessary to be measured when products leave factories, and the moisture content of the AP is required to be less than or equal to 0.05 percent.
At present, the method for detecting the water content of ammonium perchlorate mainly adopts a standard method: oven method and Karl Fischer method, but the oven analysis time is long (about 3 hours, 105 ℃), Karl Fischer method has destructive, complicated operation, and long analysis time (more than 12 hours). These two methods do not provide real-time feedback to guide the moisture content information during the AP production process.
The terahertz spectrum technology has the characteristics of safety, rapidness and nondestructive detection, and the moisture has strong absorption to terahertz, so that numerous researchers have developed the research on the detection of the moisture content in substances by utilizing the terahertz technology, and obtain good results. Before terahertz spectrum detects ammonium perchlorate moisture content, need earlier through detecting the ammonium perchlorate standard sample of different moisture contents and drawing the standard curve. The even distribution of moisture in the ammonium perchlorate standard sample is the key of guaranteeing terahertz spectrum testing result, and if moisture is uneven in the sample, the accuracy greatly reduced that terahertz spectrum detected can make.
Disclosure of Invention
In view of this, the present invention aims to provide a method for preparing standard ammonium perchlorate samples with different water contents. The ammonium perchlorate standard sample obtained by the method is uniform in water distribution, and the stability and accuracy of measuring the water content of the ammonium perchlorate by the terahertz spectroscopy can be guaranteed.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of ammonium perchlorate standard samples with different water contents, which comprises the following steps:
(1) providing a low-moisture-content ammonium perchlorate standard sample with the moisture content of 1-2 wt%, and comprising the following steps:
(a) completely spreading the dried ammonium perchlorate powder in a sample box body, and mechanically pressing to obtain an ammonium perchlorate sheet;
(b) spraying water mist into the ammonium perchlorate slice to enable the total mass of the sample box body and the hydrous ammonium perchlorate to be higher than the set total mass, covering the sample box cover body, standing for more than 10 hours, opening the sample box cover body, drying the ammonium perchlorate slice until the total mass of the sample box body and the ammonium perchlorate reaches the set total mass, covering the sample box cover body, and standing for 40-60 minutes to obtain an ammonium perchlorate standard sample with low moisture content;
the set total mass is calculated according to formula 1:
in formula 1, mtotalSetting the total mass g of the sample box body and the hydrous ammonium perchlorate;
mAPis driedMass of dried ammonium perchlorate powder, g;
msample boxMass of the sample cartridge body, g;
Pwater (W)The water content of the ammonium perchlorate standard sample is percent;
(2) sequentially drying and standing the ammonium perchlorate standard sample with low moisture content obtained in the step (1), and reducing the moisture content of the ammonium perchlorate standard sample in a gradient manner to obtain the ammonium perchlorate standard sample with low moisture content and different water contents; the standing time is 40-60 min;
(3) providing a standard ammonium perchlorate sample with a high moisture content of 5-15 wt%, which comprises the following steps:
(i) completely spreading the completely dried ammonium perchlorate powder in the sample box body;
(ii) spraying water mist into the ammonium perchlorate to enable the total mass of the sample box body and the ammonium perchlorate containing water to be higher than the set total mass, covering the sample box cover body, standing for more than 3h, opening the sample box cover body, drying the ammonium perchlorate until the total mass of the sample box body and the ammonium perchlorate reaches the set total mass, covering the sample box cover body, and standing for 30-50 min to obtain an ammonium perchlorate standard sample with high moisture content; the set total mass is calculated according to formula 1;
(4) sequentially drying and standing the ammonium perchlorate standard sample with high moisture content obtained in the step (3), and reducing the moisture content of the ammonium perchlorate standard sample in a gradient manner to obtain the ammonium perchlorate standard sample with high moisture content and different water contents; the standing time is 30-50 min.
Preferably, the sample box body and the sample box cover body are made of polytetrafluoroethylene.
Preferably, the particle size of the ammonium perchlorate powder is 5-34 mu m.
Preferably, the inner diameter of the sample box body is 30-42 mm; when preparing a low-moisture ammonium perchlorate standard sample with the moisture content of 1-2 wt%, the depth of the sample box body is 4-6 mm; when the water content is 5-15 wt% of the high-water-content ammonium perchlorate standard sample, the depth of the sample box body is 2.5-3.5 mm.
Preferably, when preparing a low-moisture ammonium perchlorate standard sample with the moisture content of 1-2 wt%, the mass of the ammonium perchlorate powder is 1.5-6 g;
when preparing a high-moisture ammonium perchlorate standard sample with a moisture content of 5-15 wt%, the mass of the ammonium perchlorate powder is 1.5-3 g.
Preferably, the pressure of the mechanical pressing is 4-5 tons, and the time is 3-5 min.
Preferably, the water content of the ammonium perchlorate in the sample box after the water mist is sprayed in the steps (b) and (ii) is 1-3% higher than that of the standard ammonium perchlorate sample.
Preferably, the drying temperature in the steps (1) - (4) is 55-65 ℃.
The invention provides application of the ammonium perchlorate standard samples with different water contents prepared by the preparation method as standard samples for measuring the water content of the ammonium perchlorate by terahertz spectroscopy.
The invention provides a preparation method of ammonium perchlorate standard samples with different water contents, which fully considers the relationship between the porosity and the water content of ammonium perchlorate powder, and adopts different modes to prepare the ammonium perchlorate standard samples according to the difference of the water contents, in particular, when the water content of the ammonium perchlorate standard samples is 1-2 wt%, the invention adopts a mechanical pressing mode to reduce the porosity among dried ammonium perchlorate powder, thereby ensuring that less water is uniformly distributed in the ammonium perchlorate; when the moisture content of the ammonium perchlorate standard sample is 5-15 wt%, the method adopts a mode of flatly paving the dried ammonium perchlorate in the sample box, so that high porosity among ammonium perchlorate powder can be ensured, and more moisture is uniformly distributed in the ammonium perchlorate without overflowing; according to the method, the influence of the standing time on the water diffusion is fully considered, the uniform diffusion of water among the pores of the ammonium perchlorate powder can be ensured by limiting the standing time in the preparation process of the ammonium perchlorate standard sample with different water contents, and the water in the obtained ammonium perchlorate standard sample is uniformly distributed; according to the method, the ammonium perchlorate standard sample with low moisture content and the ammonium perchlorate standard sample with high moisture content are dried and stood, the moisture content of the ammonium perchlorate standard sample is reduced in a gradient manner, and the ammonium perchlorate standard samples with different moisture contents are obtained. The results of the examples show that the terahertz spectrum of the standard sample prepared by the invention is very stable, which indicates that the moisture distribution in the standard sample is uniform.
The method can be used for preparing the ammonium perchlorate standard samples with different gradient water contents and can be used as the standard sample for measuring the water content of the ammonium perchlorate by terahertz spectroscopy. The standard sample prepared by the method is uniform in water distribution, and the accuracy of measuring the water content of the ammonium perchlorate by the terahertz spectrum can be ensured.
Drawings
FIG. 1 is a spectrum of absorption coefficient of a polytetrafluoroethylene material in a terahertz wave band;
FIG. 2 is a pictorial view of a sample cartridge body and a sample cartridge cover;
FIG. 3 is a pictorial representation of a briquette;
FIG. 4 is a terahertz spectrum of an ammonium perchlorate sample with a moisture content of 1 wt% at different standing times;
FIG. 5 is a terahertz spectrum of an ammonium perchlorate sample with a moisture content of 5 wt% at different standing times;
FIG. 6 is a diagram of the change of a terahertz time-domain spectrum of a sample sprayed with water mist in the standing process;
fig. 7 is a graph of the change of the terahertz time-domain spectrum of the dried sample during standing.
Detailed Description
The invention provides a preparation method of ammonium perchlorate standard samples with different water contents, which comprises the following steps:
(1) providing a low-moisture-content ammonium perchlorate standard sample with the moisture content of 1-2 wt%, and comprising the following steps:
(a) and (4) spreading the oven-dried ammonium perchlorate powder in the sample box body, and performing mechanical pressing to obtain an ammonium perchlorate sheet.
In the present invention, the material of the sample cartridge body and the cover is preferably polytetrafluoroethylene. The absorption coefficient of the polytetrafluoroethylene material is lower than that of other materials (such as acrylic, polystyrene, polypropylene or polyvinyl chloride), and no obvious absorption peak exists, so that the detection of the terahertz spectrum on the moisture of the ammonium perchlorate is facilitated.
In the present invention, the inner diameter of the cartridge body is preferably 40 mm; the depth of the sample cartridge body is preferably 5 mm. In the present invention, the sample cartridge cover has a cylindrical protrusion surface, and the size of the cylindrical protrusion is adapted to the inner diameter of the sample cartridge. When the terahertz spectrum of the ammonium perchlorate standard sample is tested, the sample box cover body covers the sample box body.
In the invention, when the diameter of the sample box body is 40mm and the depth is 5mm, the mass of the ammonium perchlorate is preferably 1.5-6 g, and more preferably 2-4 g.
In the present invention, the method of mechanical compression is preferably compression by a tablet press. The pressure of the mechanical pressing is preferably 4-5 tons, and more preferably 4.5 tons; the time is preferably 3 to 5min, and more preferably 4 min. The invention can reduce the porosity among the dried ammonium perchlorate powder by mechanical pressing, thereby ensuring that less moisture is uniformly distributed in the ammonium perchlorate.
(b) Spraying water mist into the ammonium perchlorate slice to enable the total mass of the sample box body and the hydrous ammonium perchlorate to be higher than the set total mass, covering the sample box cover body, and standing for more than 10 hours; and opening the sample box cover body, drying the ammonium perchlorate slice until the total mass of the sample box body and the ammonium perchlorate reaches the set total mass, covering the sample box cover body, standing for 40-60 min, and obtaining the ammonium perchlorate standard sample with low moisture content.
In the invention, the spraying equipment used in spraying the water mist is preferably a spraying bottle, and the distance between a spraying nozzle used in spraying the water mist and the ammonium perchlorate is 30-50 cm, and the distance between the spraying nozzle and the ammonium perchlorate is preferably 35-45 cm.
In the invention, the water content of the ammonium perchlorate in the sample box after the water mist is sprayed in the step (b) is 1-3% higher than that of the ammonium perchlorate standard sample, and the water content is more preferably 2%.
In the invention, after the water mist is sprayed, the standing time is not less than 10 hours, preferably 10-20 hours, and more preferably 12-15 hours. In the present invention, the standing is preferably performed at room temperature, and the present invention enables uniform diffusion of moisture in the ammonium perchlorate flakes by the standing.
In the invention, the drying mode is preferably oven drying, and the drying temperature is preferably 55-65 ℃, more preferably 58-62 ℃, and more preferably 60 ℃.
In the invention, the standing time after drying is 40-60 min, preferably 45-55 min, and more preferably 50 min. In the drying process, the moisture on the surface of the ammonium perchlorate standard sample is lost firstly, so that the moisture is unevenly distributed; according to the invention, through the standing, the moisture is uniformly diffused in the dried ammonium perchlorate again.
In the present invention, the set total mass is calculated according to formula 1:
in formula 1, mtotalSetting the total mass g of the sample box body and the hydrous ammonium perchlorate;
mAPmass of dried ammonium perchlorate powder, g;
msample boxMass of the sample cartridge body, g;
Pwater (W)The water content of the ammonium perchlorate standard sample is percent;
in the present invention, the formula 1 is derived from the formula a and the formula B:
mtotal＝mAP+mPTFE+mwaterformula B;
in the formulae A and B, PwaterThe water content of the ammonium perchlorate standard sample is percent;
mwatermass of water, g;
mtotalsetting the total mass g of the sample box body and the hydrous ammonium perchlorate;
mAPmass of dried ammonium perchlorate, g;
mPTFEis the mass of the cartridge body, g.
(2) Sequentially drying and standing the ammonium perchlorate standard sample with low moisture content obtained in the step (1), and reducing the moisture content of the ammonium perchlorate standard sample in a gradient manner to obtain the ammonium perchlorate standard sample with low moisture content and different water contents; the standing time is 40-60 min.
In the invention, the drying mode is preferably oven drying, and the drying temperature is preferably 55-65 ℃, more preferably 58-62 ℃, and more preferably 60 ℃.
In the invention, the standing time after drying is 40-60 min, more preferably 45-55 min, and still more preferably 50 min.
As a specific embodiment of the present invention, the step of reducing the moisture content of the ammonium perchlorate standard sample preferably comprises the following steps:
obtaining a low-moisture ammonium perchlorate standard sample with the moisture content of 1 wt% according to the step (1);
setting the water content of the ammonium perchlorate standard sample to be 0.9%, 0.8%, 0.7%, 0.6%, 0.5%, 0.4%, 0.3%, 0.2%, 0.1% and 0%, drying the ammonium perchlorate standard sample with the water content of 1% until the total mass of the sample box body and the ammonium perchlorate reaches the set total mass, covering the sample box cover, standing to obtain the ammonium perchlorate standard sample with the water content of 0.9%, and calculating the set total mass according to formula 1. In the invention, the drying mode is preferably oven drying, and the drying temperature is preferably 55-65 ℃, more preferably 58-62 ℃, and more preferably 60 ℃; and after drying, the standing time is more than or equal to 40min, preferably 40-60 min, and more preferably 45-55 min.
Drying the ammonium perchlorate standard sample with the water content of 0.9 percent until the total mass of the sample box body and the ammonium perchlorate reaches the set total mass, covering the sample box cover, standing to obtain the ammonium perchlorate standard sample with the water content of 0.8 percent, and calculating the set total mass according to the formula 1. In the invention, the drying mode is preferably oven drying, and the drying temperature is preferably 55-65 ℃, more preferably 58-62 ℃, and more preferably 60 ℃; and after drying, the standing time is more than or equal to 40min, preferably 40-60 min, and more preferably 45-55 min.
By analogy, ammonium perchlorate samples with water contents of 0.9%, 0.8%, 0.7%, 0.6%, 0.5%, 0.4%, 0.3%, 0.2%, 0.1% and 0% were obtained.
(3) Providing a standard ammonium perchlorate sample with a high moisture content of 5-15 wt%, which comprises the following steps:
(i) and spreading the oven-dried ammonium perchlorate powder in the sample box body.
In the present invention, the particle size, purity and drying manner of the ammonium perchlorate powder are within the scope of the preparation method above, and are not described in detail herein.
In the present invention, the inner diameter of the cartridge body is preferably 40 mm; the depth of the sample cartridge body is preferably 3 mm. In the invention, when the inner diameter of the sample box body is 40mm and the depth is 3mm, the mass of the ammonium perchlorate is preferably 1.5-3 g, and more preferably 2-2.5 g. In the present invention, the structure of the cover of the sample cartridge is preferably the same as that described above, and will not be described herein.
After the ammonium perchlorate powder is flatly paved, the flatly paved ammonium perchlorate powder is preferably lightly pressed by a pressing block so as to ensure the flatness of the flatly paved ammonium perchlorate powder. In the invention, the material of the briquetting is preferably polytetrafluoroethylene; the pressing block is preferably cylindrical in shape, and the diameter of the pressing block is matched with the inner diameter of the box body of the sample box. In the present invention, the height of the compact is preferably greater than the depth of the sample cartridge body.
(ii) Spraying water mist into the ammonium perchlorate to enable the total mass of the sample box body and the ammonium perchlorate containing water to be higher than the set total mass, covering the sample box cover body, standing for more than 3h, opening the sample box cover body, drying the ammonium perchlorate until the total mass of the sample box body and the ammonium perchlorate reaches the set total mass, covering the sample box cover body, and standing for 30-50 min to obtain an ammonium perchlorate standard sample with high moisture content; the set total mass is calculated according to formula 1;
in the present invention, the manner of spraying the water mist is within the scope of the above preparation method, and is not described herein again.
In the invention, the water content of the ammonium perchlorate in the sample box after the water mist is sprayed in the step (ii) is 1-3% higher than that of the ammonium perchlorate standard sample, and the water content is more preferably 2%.
In the invention, after the water mist is sprayed, the standing time is not less than 3 hours, preferably 3-6 hours, and more preferably 4-5 hours. In the present invention, the standing is preferably performed at room temperature, and the present invention enables uniform diffusion of moisture in the ammonium perchlorate flakes by the standing.
In the invention, the drying mode is preferably oven drying, and the drying temperature is preferably 55-65 ℃, more preferably 58-62 ℃, and more preferably 60 ℃.
In the invention, the standing time after drying is 30-50 min, preferably 35-45 min, and more preferably 40 min. In the drying process, the moisture on the surface of the ammonium perchlorate standard sample is lost firstly, so that the moisture is unevenly distributed; according to the invention, through the standing, the moisture is uniformly diffused in the dried ammonium perchlorate again.
(4) Sequentially drying and standing the ammonium perchlorate standard sample with high moisture content obtained in the step (3), and reducing the moisture content of the ammonium perchlorate standard sample in a gradient manner to obtain the ammonium perchlorate standard sample with high moisture content and different water contents; the standing time is 30-50 min.
As a specific embodiment of the present invention, the step of reducing the moisture content of the ammonium perchlorate standard sample preferably comprises the following steps:
obtaining a low-moisture ammonium perchlorate standard sample with the moisture content of 6 wt% according to the step (1);
the method comprises the steps of setting the water content of an ammonium perchlorate standard sample to be 5.5%, 5%, 4.5%, 4%, 3.5%, 3%, 2.5%, 2% and 1.5%, drying the ammonium perchlorate standard sample with the water content of 6% until the total mass of a sample box body and ammonium perchlorate reaches the set total mass, covering a sample box cover, standing to obtain the ammonium perchlorate standard sample with the water content of 5.5%, and calculating the set total mass according to formula 1. In the invention, the drying mode is preferably oven drying, and the drying temperature is preferably 55-65 ℃, more preferably 58-62 ℃, and more preferably 60 ℃; and after drying, the standing time is 30-50 min, preferably 35-45 min, and more preferably 40 min.
Drying the ammonium perchlorate standard sample with the water content of 5.5 percent until the total mass of the sample box body and the ammonium perchlorate reaches the set total mass, covering the sample box cover, standing to obtain the ammonium perchlorate standard sample with the water content of 5 percent, and calculating the set total mass according to the formula 1. In the invention, the drying mode is preferably oven drying, and the drying temperature is preferably 55-65 ℃, more preferably 58-62 ℃, and more preferably 60 ℃; and after drying, the standing time is 30-50 min, preferably 35-45 min, and more preferably 40 min.
By analogy, 5.5%, 5%, 4.5%, 4%, 3.5%, 3%, 2.5%, 2%, 1.5% ammonium perchlorate standard samples were obtained.
The invention provides application of the ammonium perchlorate standard samples with different water contents prepared by the preparation method as standard samples for measuring the water content of the ammonium perchlorate by terahertz spectroscopy.
The following examples are provided to illustrate the preparation of standard ammonium perchlorate samples with different water contents according to the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
(one) preparation of a Standard sample having an ammonium perchlorate moisture content of 1 wt%
(1) Taking 6g of dried ammonium perchlorate powder with the particle size of 5-34 mu m and the purity of 99.5%, flatly paving the ammonium perchlorate powder in a polytetrafluoroethylene sample box body, wherein the inner diameter of the sample box body is 40mm, the depth of the sample box body is 5mm, and pressing the ammonium perchlorate powder for 4min by using a 4-ton tablet press to obtain an ammonium perchlorate sheet;
(2) and spraying water mist into the ammonium perchlorate slice to ensure that the total mass of the sample box body and the hydrous ammonium perchlorate is higher than the set total mass, covering the sample box cover body, and standing for 10 hours.
The absorption coefficient spectrogram and the refraction spectrogram of the box body of the polytetrafluoroethylene sample box in the terahertz wave band are shown in figure 1, the absorption coefficient of the box body in the terahertz wave band is low, no obvious absorption peak exists, and the box body can be used for detecting the moisture of the ammonium perchlorate by the terahertz spectrum.
The real object diagram of the box body and the cover body of the polytetrafluoroethylene sample box is shown in figure 2, the left side is the box body of the sample box, and the right side is the cover body.
The change of the terahertz time-domain spectrum of the sample sprayed with the water mist in the standing process is shown in fig. 4. In fig. 4, (a) is a variation diagram of the terahertz time-domain spectrum, and (b) is a partially enlarged diagram. As can be seen from fig. 4, the low water content sample tends to be stable at 10h, i.e., the water distribution is uniform.
(3) And opening the sample box cover body, drying the ammonium perchlorate slice at the drying temperature of 60 ℃ until the total mass of the sample box body and the ammonium perchlorate reaches the set total mass, covering the sample box cover body, and standing for 40min to obtain the ammonium perchlorate standard sample with low moisture content.
Wherein, the change of the terahertz time-domain spectrum of the dried sample in the standing process is shown in fig. 5. In fig. 5, (a) is a variation diagram of the terahertz time-domain spectrum, and (b) is a partially enlarged diagram. As can be seen from fig. 5, the low water content sample tends to stabilize after 40 min.
And (II) reducing the water content of the standard sample with the water content of 1 wt% by drying in an oven and the like in a gradient manner to obtain ammonium perchlorate samples with the water contents of 0.9%, 0.8%, 0.7%, 0.6%, 0.5%, 0.4%, 0.3%, 0.2%, 0.1% and 0%. The temperature for each drying is 60 deg.C, and the standing time is 40 min.
(III) preparation of a Standard sample having a moisture content of ammonium perchlorate of 6 wt%
(a) 3g of dried ammonium perchlorate powder with the particle size of 5-34 mu m and the purity of 99.5 percent is flatly paved in a sample box body, the inner diameter of the sample box body is 40mm, the depth of the sample box body is 3mm, a polytetrafluoroethylene pressing block is used for flattening when the sample box body is flatly paved, and a real object diagram of the polytetrafluoroethylene pressing block is shown in figure 3.
(b) And spraying water mist into the ammonium perchlorate to ensure that the total mass of the sample box body and the hydrous ammonium perchlorate is higher than the set total mass, covering the sample box cover body and standing for 3 hours.
The change of the terahertz time-domain spectrum of the sample sprayed with the water mist in the standing process is shown in fig. 6. In fig. 6, (a) is a variation diagram of the terahertz time-domain spectrum, and (b) is a partially enlarged diagram. As can be seen from FIG. 6, the high water content sample tends to be stable in 3h, i.e., the water distribution is uniform.
(c) Opening the sample box cover body, drying the ammonium perchlorate until the total mass of the sample box body and the ammonium perchlorate reaches the set total mass, covering the sample box cover body, and standing for 30min to obtain an ammonium perchlorate standard sample with high moisture content; the set total mass is calculated according to formula 1.
The change of the terahertz time-domain spectrum of the dried sample in the standing process is shown in fig. 7. In fig. 7, (a) is a variation diagram of the terahertz time-domain spectrum, and (b) is a partially enlarged diagram. As can be seen from fig. 7, the low water content sample tends to stabilize after 30 min.
And (IV) reducing the water content of the standard sample with the water content of 6 wt% by drying in an oven and the like in a gradient manner to obtain the standard sample of ammonium perchlorate with the water content of 5.5%, 5%, 4.5%, 4%, 3.5%, 3%, 2.5%, 2% and 1.5%. The temperature for each drying is 60 deg.C, and the standing time is 30 min.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A preparation method of ammonium perchlorate standard samples with different water contents comprises the following steps:
(1) providing a low-moisture-content ammonium perchlorate standard sample with the moisture content of 1-2 wt%, and comprising the following steps:
(a) completely spreading the dried ammonium perchlorate powder in a sample box body, and mechanically pressing to obtain an ammonium perchlorate sheet;
(b) spraying water mist into the ammonium perchlorate slice to enable the total mass of the sample box body and the hydrous ammonium perchlorate to be higher than the set total mass, covering the sample box cover body, standing for more than 10 hours, opening the sample box cover body, drying the ammonium perchlorate slice until the total mass of the sample box body and the ammonium perchlorate reaches the set total mass, covering the sample box cover body, and standing for 40-60 minutes to obtain an ammonium perchlorate standard sample with low moisture content;
the set total mass is calculated according to formula 1:
in formula 1, mtotalSetting the total mass g of the sample box body and the hydrous ammonium perchlorate;
mAPmass of dried ammonium perchlorate powder, g;
msample boxMass of the sample cartridge body, g;
Pwater (W)The water content of the ammonium perchlorate standard sample is percent;
(2) sequentially drying and standing the ammonium perchlorate standard sample with low moisture content obtained in the step (1), and reducing the moisture content of the ammonium perchlorate standard sample in a gradient manner to obtain the ammonium perchlorate standard sample with low moisture content and different water contents; the standing time is 40-60 min;
(3) providing a standard ammonium perchlorate sample with a high moisture content of 5-15 wt%, which comprises the following steps:
(i) completely spreading the completely dried ammonium perchlorate powder in the sample box body;
(ii) spraying water mist into the ammonium perchlorate to enable the total mass of the sample box body and the ammonium perchlorate containing water to be higher than the set total mass, covering the sample box cover body, standing for more than 3h, opening the sample box cover body, drying the ammonium perchlorate until the total mass of the sample box body and the ammonium perchlorate reaches the set total mass, covering the sample box cover body, and standing for 30-50 min to obtain an ammonium perchlorate standard sample with high moisture content; the set total mass is calculated according to formula 1;
(4) sequentially drying and standing the ammonium perchlorate standard sample with high moisture content obtained in the step (3), and reducing the moisture content of the ammonium perchlorate standard sample in a gradient manner to obtain the ammonium perchlorate standard sample with high moisture content and different water contents; the standing time is 30-50 min.
2. The method of claim 1, wherein the sample cartridge body and the sample cartridge cover are made of polytetrafluoroethylene.
3. The method according to claim 1, wherein the ammonium perchlorate powder has a particle size of 5 to 34 μm.
4. The preparation method according to claim 1 or 2, wherein the inner diameter of the cartridge body is 30 to 42 mm; when preparing a low-moisture ammonium perchlorate standard sample with the moisture content of 1-2 wt%, the depth of the sample box body is 4-6 mm; when the water content is 5-15 wt% of the high-water-content ammonium perchlorate standard sample, the depth of the sample box body is 2.5-3.5 mm.
5. The method according to claim 4, wherein when preparing a low moisture content ammonium perchlorate standard sample having a moisture content of 1 to 2 wt%, the ammonium perchlorate powder has a mass of 1.5 to 6 g;
when preparing a high-moisture ammonium perchlorate standard sample with a moisture content of 5-15 wt%, the mass of the ammonium perchlorate powder is 1.5-3 g.
6. The method according to claim 1 or 5, wherein the mechanical pressing is performed under a pressure of 4 to 5 tons for 3 to 5 minutes.
7. The preparation method according to claim 1, wherein the water content of the ammonium perchlorate in the sample box sprayed with the water mist in the steps (b) and (ii) is 1-3% higher than that of the standard ammonium perchlorate sample.
8. The method according to claim 1, wherein the drying temperature in the steps (1) to (4) is 55 to 65 ℃.
9. The application of the ammonium perchlorate standard samples with different water contents prepared by the preparation method of any one of claims 1 to 8 as standard samples for measuring the water content of ammonium perchlorate by terahertz spectroscopy.
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| CN202110101536.2A CN112683841B (en) | 2021-01-26 | 2021-01-26 | Preparation method of ammonium perchlorate standard samples with different water contents |
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