CN110987734B - Solid washing material of dry-method laser particle size analyzer and cleaning method thereof - Google Patents

Solid washing material of dry-method laser particle size analyzer and cleaning method thereof Download PDF

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CN110987734B
CN110987734B CN201911269442.5A CN201911269442A CN110987734B CN 110987734 B CN110987734 B CN 110987734B CN 201911269442 A CN201911269442 A CN 201911269442A CN 110987734 B CN110987734 B CN 110987734B
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particle size
cleaning
dry
laser particle
size analyzer
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CN110987734A (en
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罗隽
宿亮
刘科
李峥嵘
曹瑞
谭鑫强
龙世玉
陈涛
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Hunan Qianjin Xiangjiang Pharmaceutical Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/02Investigating particle size or size distribution
    • G01N15/0205Investigating particle size or size distribution by optical means, e.g. by light scattering, diffraction, holography or imaging
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning

Abstract

The invention belongs to the technical field of laser particle size analyzers, and discloses application of microcrystalline cellulose in a cleaning dry-process laser particle size analyzer. The invention also provides a method for cleaning the dry-process laser particle size analyzer by utilizing the microcrystalline cellulose, and specifically, the microcrystalline cellulose is placed in the dry-process laser particle size analyzer, and a cleaning program is started for cleaning. The invention adopts microcrystalline cellulose as the washing material of the dry-process laser particle size analyzer, can take away light materials adsorbed on pipelines and walls of the analyzer by only adopting one material under the action of airflow, has good washing effect, can be washed once, has no dust escape in the whole washing process, ensures that the dry-process laser particle size analyzer is convenient and quick to wash, and has no abrasion to the pipelines in the analyzer after long-term use.

Description

Solid washing material of dry-method laser particle size analyzer and cleaning method thereof
Technical Field
The invention belongs to the technical field of laser particle size analyzers. And more particularly, to a solid washing material for a dry laser particle size analyzer and a washing method thereof.
Background
When a laser particle size analyzer is used for dry determination of materials which are light in weight, low in density, easy to adsorb and poor in flowability, if the materials in an instrument pipeline are not cleaned up, secondary test results of the materials can be affected, for example, shoulder peaks, tailing and the like can appear in a particle size spectrum, and the repeatability of detection is poor. Therefore, finding the cleaning material suitable for the dry-process laser particle size analyzer has important significance for ensuring the accuracy of the dry-process determination of the laser particle size analyzer.
The patent CN106370566B provides a solid washing material of a dry-process laser particle size analyzer comprising barium sulfate and quartz powder, and a method for cleaning the dry-process laser particle size analyzer by utilizing the solid washing material. However, the barium sulfate in the solid washing material provided by the invention is a material with a large specific gravity (about 4.5), and the residual substances are mainly taken away by utilizing the gravity action of the barium sulfate, so that the risk that the barium sulfate abrades the pipeline of the laser particle analyzer and the mirror surface of the detector exists in the process; in addition, the solid washing material has more components, and needs to be further washed by adopting an auxiliary surfactant, so that the washing effect of the single solid washing material of barium sulfate is not the washing effect of the single solid washing material of barium sulfate, the raw materials need to be mixed according to a certain proportion, the washing times are more, and the operation is troublesome.
Therefore, the method for cleaning the dry-method laser particle size analyzer, which has the advantages of simple process, high cleaning efficiency and no damage to the instrument, is found to have important application value.
Disclosure of Invention
The invention aims to provide a solid washing material of a dry-process laser particle size analyzer and a cleaning method thereof, wherein the washing material consists of microcrystalline cellulose, and light materials adsorbed on a pipeline and a wall of the analyzer can be taken away by only one material under the action of airflow, so that the apparatus is free from damage, the cleaning effect is good, the cleaning effect can be achieved by cleaning once, no dust escapes in the whole cleaning process, and the dry-process laser particle size analyzer is convenient and quick to clean.
The invention aims to provide application of microcrystalline cellulose in cleaning a dry-method laser particle size analyzer.
It is another object of the present invention to provide the use of microcrystalline cellulose as a wash stock for a dry laser particle size analyzer.
Still another object of the present invention is to provide a solid purge for a dry laser particle size analyzer.
It is yet another object of the present invention to provide a method of cleaning a dry laser particle size analyzer.
The above purpose of the invention is realized by the following technical scheme:
the invention provides application of microcrystalline cellulose in cleaning a dry laser particle size analyzer.
The invention also provides application of the microcrystalline cellulose in washing materials used as a dry-process laser particle size analyzer.
Preferably, the microcrystalline cellulose has an average particle size of 60 to 250 μm.
The microcrystalline cellulose is a natural high molecular compound, is white, odorless and tasteless, is nontoxic and non-irritant crystalline powder consisting of porous particles, is easy to adsorb other materials, has good fluidity and small specific gravity of only 1.5, and hardly wears instruments. And the material is easily purchased in the market.
The invention also provides a solid washing material of the dry-process laser particle size analyzer, which consists of the microcrystalline cellulose.
Preferably, the microcrystalline cellulose has an average particle size of 60 to 250 μm.
In addition, the method for cleaning the dry laser particle size analyzer by using the solid washing material is also within the protection scope of the invention.
Preferably, the method is to place the microcrystalline cellulose in a dry laser particle size analyzer and start a cleaning procedure for cleaning.
Preferably, the dosage of the solid washing material is 0.5-1.0g.
Preferably, the inlet pressure of the washing procedure is 2 to 4bar.
Preferably, the sample injection speed of the cleaning is 30-60%.
Most preferably, the purge has a feed gas pressure of 3bar and a feed rate of 50%.
When the microcrystalline cellulose is used for cleaning the dry-method laser particle size analyzer, an excellent cleaning effect can be obtained by cleaning once, the result repeatability of the particle size of the sample tested by the cleaned particle size analyzer is good, the operation is quick and convenient, and the method has important application value in the fields of scientific research, detection and the like.
The invention has the following beneficial effects:
the material for washing provided by the invention can take away the light materials adsorbed on the pipeline and the wall of the dry-process laser particle size analyzer through only one material, so that the instrument is not damaged, the washing effect is good, the material can be washed once, no dust escapes in the whole washing process, and the dry-process laser particle size analyzer is convenient and quick to wash.
Drawings
FIG. 1 is a diagram of a first test using a dry laser particle size analyzer;
FIG. 2 is a diagram of a second test performed after a conventional cleaning of a dry laser particle size analyzer;
fig. 3 is a spectrum of a third detection performed after the microcrystalline cellulose washing material of the present invention is washed by a dry laser particle size analyzer.
FIG. 4 is a graph of a first test using a dry laser particle size analyzer;
FIG. 5 is a spectrum of a second detection performed after a first cleaning of a dry laser particle analyzer by a barium sulfate mixture;
fig. 6 is a graph showing a third detection performed after a dry laser particle size analyzer was washed three times with a barium sulfate mixture.
Detailed Description
The invention is further described with reference to the drawings and the following detailed description, which are not intended to limit the invention in any way.
Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1 laser particle size detection of amlodipine besylate
1. Amlodipine besylate granularity detection
The cleaning procedure parameters were as follows:
dispersion air pressure (intake air pressure): 3.0bar;
sample introduction speed: 50 percent.
After the parameters are set, a proper amount of amlodipine besylate is placed in a dry laser particle size analyzer, and detection is started. The amlodipine besylate is light and easy to adhere to the pipeline, so the pipeline needs to be cleaned.
2. Cleaning method
(1) Conventional cleaning
And directly starting a cleaning program of the dry-process laser particle size analyzer for cleaning.
(2) Microcrystalline cellulose cleaning
1g of microcrystalline cellulose (with the average particle size of 60-250 μm) is placed in a dry-process laser particle size analyzer, and a cleaning program of the dry-process laser particle size analyzer is started for cleaning, so that the third particle size detection of the amlodipine besylate can be performed.
3. The result of the detection
Fig. 1 is a spectrum of a first detection performed by a dry laser particle size analyzer, fig. 2 is a spectrum of a second detection performed after a conventional cleaning of the dry laser particle size analyzer, and fig. 3 is a spectrum of a third detection performed after a cleaning of the dry laser particle size analyzer by a microcrystalline cellulose washing material according to the present invention. The results of the sample detection after washing by the two washing methods obtained by comparing the three spectra are shown in table 1.
TABLE 1
Figure BDA0002313760230000041
The spectra of the three detections show that the first detection result is equivalent to the third detection result, and the second detection result has obvious tailing, so that the parameter values are increased in different degrees. Compared with the conventional method, after the pipeline of the particle analyzer is cleaned by microcrystalline cellulose, the particle size detection spectrum of the sample is obviously improved, and has no obvious difference with the first measurement result. The microcrystalline cellulose cleaning effect is excellent, and the result repeatability of the test sample of the particle size analyzer after cleaning is good.
Example 2 laser particle size detection of amlodipine besylate
1. Amlodipine besylate particle size detection
The cleaning procedure parameters were as follows:
dispersing air pressure: 2.0bar;
sample introduction speed: 30 percent.
After the parameters are set, a proper amount of amlodipine besylate is placed in a dry laser particle size analyzer, and detection is started. The amlodipine besylate is light and easy to adhere to the pipeline, so the pipeline needs to be cleaned.
2. Cleaning method
(1) Conventional cleaning
And directly starting a cleaning program of the dry-method laser particle size analyzer for cleaning.
(2) Microcrystalline cellulose cleaning
1g of microcrystalline cellulose (with the average particle size of 60-250 μm) is placed in a dry-process laser particle size analyzer, and a cleaning program of the dry-process laser particle size analyzer is started for cleaning, so that the third particle size detection of the amlodipine besylate can be performed.
3. The detection results show that the first detection result is equivalent to the third detection result in the three detection spectrums, and the second detection result has obvious tailing, so that the parameter values are increased in different degrees. Compared with the conventional method, after the pipeline of the particle size analyzer is cleaned by microcrystalline cellulose, the particle size detection spectrum of the sample is obviously improved, and the difference with the first measurement result is not obvious. The microcrystalline cellulose cleaning effect is excellent, and the result repeatability of the sample tested by the particle size analyzer after cleaning is good.
Example 3 laser particle size detection of amlodipine besylate
1. Amlodipine besylate particle size detection
The cleaning program parameters were as follows:
dispersing air pressure: 4.0bar;
sample introduction speed: 60 percent.
After the parameters are set, a proper amount of amlodipine besylate is placed in a dry laser particle size analyzer, and detection is started. The amlodipine besylate is light and easy to adhere to the pipeline, so the pipeline needs to be cleaned.
2. Cleaning method
(1) Conventional cleaning
And directly starting a cleaning program of the dry-process laser particle size analyzer for cleaning.
(2) Microcrystalline cellulose cleaning
1g of microcrystalline cellulose (with the average particle size of 60-250 μm) is placed in a dry-process laser particle size analyzer, and a cleaning program of the dry-process laser particle size analyzer is started for cleaning, so that the third particle size detection of the amlodipine besylate can be performed.
3. The detection results show that the first detection result is equivalent to the third detection result in the three detection spectrums, and the second detection result has obvious tailing, so that the parameter values are increased in different degrees. Compared with the conventional method, after the pipeline of the particle size analyzer is cleaned by microcrystalline cellulose, the particle size detection spectrum of the sample is obviously improved, and the difference with the first measurement result is not obvious. The microcrystalline cellulose cleaning effect is excellent, and the result repeatability of the sample tested by the particle size analyzer after cleaning is good.
Comparative example 1
1. Amlodipine besylate granularity detection
The cleaning program parameters were as follows:
dispersion air pressure (intake air pressure): 2.0bar;
sample introduction speed: 30 percent.
After the parameters are set, a proper amount of amlodipine besylate is placed in a dry laser particle size analyzer, and detection is started. Since amlodipine besylate is light and easily adhered to the pipe, the pipe needs to be cleaned.
2. Cleaning method
(1) Cleaning the barium sulfate mixture once
0.6g of barium sulfate, 0.4g of quartz powder and 0.1g of surfactant are placed in a dry-process laser particle size analyzer, and a cleaning program of the dry-process laser particle size analyzer is started for carrying out primary cleaning, so that secondary particle size detection of the amlodipine besylate can be carried out.
(2) Barium sulfate mixture is washed three times
And (3) placing 0.6g of barium sulfate, 0.4g of quartz powder and 0.1g of surfactant in a dry-process laser particle size analyzer, starting a cleaning program of the dry-process laser particle size analyzer to carry out three times of cleaning, and then carrying out third time of particle size detection on the amlodipine besylate.
3. The result of the detection
Fig. 4 is a graph of a first detection performed by a dry laser particle size analyzer, fig. 5 is a graph of a second detection performed after a first cleaning of a barium sulfate mixture performed by the dry laser particle size analyzer, and fig. 6 is a graph of a third detection performed after a third cleaning performed by the barium sulfate mixture. The results of the sample detection after washing by the two washing methods obtained by comparing the three spectra are shown in table 2.
TABLE 2
Figure BDA0002313760230000061
The three detection results are different from one another, the detection result is obviously trailing after the barium sulfate is adopted for cleaning once before the second detection, and the parameter values are increased in different degrees, namely the effect of adopting the barium sulfate mixture for cleaning once is not ideal; the barium sulfate mixture is used for washing three times before the third detection, a slight tailing phenomenon still exists, and the effect of washing three times by using the barium sulfate mixture is still not ideal.
Comparative example 2
1. Using the method of example 1, the dry laser particle size analyzer was repeatedly washed 5 times a day and 3 times each time with microcrystalline cellulose (average particle size 60 to 250 μm) and a barium sulfate mixture (0.6 g barium sulfate, 0.4g quartz powder, and 0.1g surfactant), respectively. And (5) observing the abrasion condition of the pipeline in the instrument.
2. After 2 weeks of testing, it was found that the pipe in the apparatus was slightly worn by long-term cleaning with the barium sulfate mixture. While microcrystalline cellulose does not see any abrasion.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.

Claims (4)

1. The solid washing material of the dry-method laser particle size analyzer is characterized in that the solid washing material is microcrystalline cellulose with the average particle size of 60-250 mu m.
2. A method for cleaning a dry-process laser particle size analyzer is characterized in that microcrystalline cellulose is placed in the dry-process laser particle size analyzer, and a cleaning program is started for cleaning; the average grain size of the microcrystalline cellulose is 60-250 mu m; wherein the inlet pressure of the cleaning procedure is 2-4 bar; the sample injection speed of the cleaning is 30-60%; the dosage of the microcrystalline cellulose is 0.5-1.0g.
3. The method of claim 2, wherein the purge inlet gas pressure is 3bar.
4. The method of claim 2, wherein the cleaning is performed at a sample injection rate of 50%.
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