CN116952895A - Method for rapidly determining mixing uniformity - Google Patents
Method for rapidly determining mixing uniformity Download PDFInfo
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- CN116952895A CN116952895A CN202310915355.2A CN202310915355A CN116952895A CN 116952895 A CN116952895 A CN 116952895A CN 202310915355 A CN202310915355 A CN 202310915355A CN 116952895 A CN116952895 A CN 116952895A
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- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 14
- 238000002835 absorbance Methods 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 11
- 238000005259 measurement Methods 0.000 claims abstract description 7
- 238000005070 sampling Methods 0.000 claims abstract description 7
- 238000012935 Averaging Methods 0.000 claims abstract description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 2
- 230000003595 spectral effect Effects 0.000 claims description 2
- 238000001228 spectrum Methods 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004940 physical analysis method Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention provides a method for rapidly determining mixing uniformity, and relates to the technical field of mixing uniformity determination. The method for rapidly determining the mixing uniformity comprises the following specific steps: before measurement, sampling and collecting an original sample, collecting near infrared spectrum data of the sample through a near infrared spectrum instrument, averaging absorbance at all wavelength points of the collected sample, respectively calculating differences between absorbance at each sample wavelength and the average value, namely S1, S2..S800, and calculating the integral standard deviation, namelyCalculate coefficient of variation CV = divide the overall standard deviation S by the sample mean X and multiply by 100%, i.e.Sample uniformity at different times was analyzed by an on-line test algorithm. By adopting the infrared spectrum analysis technology, the method can not destroy samples, consume no chemical reagent, further protect the environment, and can measure different products with strong adaptability.
Description
Technical Field
The invention relates to the technical field of mixing uniformity measurement, in particular to a method for rapidly measuring mixing uniformity.
Background
Nowadays, many industries have compliance requirements on product quality and mixing uniformity, for example, the pharmaceutical industry has strict requirements on the mixing performance of medicines, the mixing uniformity is one of key factors for ensuring the product quality and performance, a method for rapidly determining the mixing uniformity can help enterprises to meet the quality control and compliance requirements, ensure the product quality and safety, simultaneously can promote process improvement and innovation, the enterprises can better understand the key factors in the mixing process by monitoring the mixing effect in real time, process improvement and optimization are carried out according to the measurement result, timely detection of the mixing effect in the production process is facilitated, and therefore rapid adjustment and optimization are realized, and the product quality and production efficiency are improved.
The traditional method for measuring the feed mixing uniformity is based on the method for measuring the feed mixing uniformity in national standard GB/T5918-2008, and takes the content of chloride ions as an example, the standard deviation S of the concentration of the chloride ions and the variation coefficient CV value of the concentration of the chloride ions are measured, and a sample is required to be detected for a certain time to obtain an accurate result, which may lead to the fact that a long time is required to be waited in actual production to obtain an evaluation result.
For this reason, we have developed a new method for rapidly determining the mixing uniformity.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a method for rapidly determining the mixing uniformity, which solves the problems that the existing mixing uniformity method needs to wait for a long time to obtain an evaluation result, has detection timeliness, cannot determine the mixing effect in real time, and is strong in limitation in determining different materials.
(II) technical scheme
In order to achieve the above purpose, the invention is realized by the following technical scheme: a method for rapidly determining the mixing uniformity comprises the following specific steps:
s1, sampling and collecting an original sample before measurement;
s2, collecting near infrared spectrum data of a sample through a near infrared spectrum instrument;
s3, averaging the absorbance of all the collected sample wavelength points;
s4, respectively calculating the difference between the absorbance and the average value of each sample wavelength, namely S1, S2..S 800;
s5, calculating the total standard deviation s=adding the standard deviations at all sample wavelengths (S1, S2..s800), and dividing by the total number of wavelengths (801), i.e.
S6, calculating a coefficient of variation cv=dividing the overall standard deviation S by the sample mean X and multiplying by 100%, i.e. cv=s/x100%;
s7, analyzing the uniformity of samples at different times through an online test algorithm;
s8, whether the standard deviation and the variation coefficient have the same trend or not is judged through an online test algorithm (standard deviation (S) and variation Coefficient (CV)), so that the mixing uniformity of the product can be timely and accurately judged.
Preferably, the original sample sampling device in S1 is an automatic rapid sample concentrator.
Preferably, the S2 near infrared spectrometer is a AvaSpec CompactLine series spectrometer, and the spectrum wavelength range of the collected sample is 900-1700nm, which is 801 wavelength points in total.
Preferably, the absorbance calculation formula in S3 isWherein A represents absorbance, I0 is light intensity before light passes through the medium, and I is light passing throughLight intensity after passing through the medium.
Preferably, the standard deviation at the wavelength in S4 is the variation degree of the spectral intensity value at each specific wavelength in the near infrared spectrum data.
Preferably, the larger the coefficient of variation in S6, the higher the relative degree of dispersion of the data, and the smaller the coefficient of variation, the lower the relative degree of dispersion of the data.
Preferably, the online test algorithm in S7 and S8 is:
input: data set x= { X1, X2,..xn }, cluster number K;
initializing K cluster centers μ1, μ2, μk;
repeating until convergence: for each data point xi, calculating the distance between each data point xi and each cluster center, selecting the nearest cluster center, classifying the data points into the clusters, and updating the cluster center as the average value of the data points of the clusters to which the data points belong;
and (3) outputting: each data point belongs to a cluster.
(III) beneficial effects
The invention provides a method for rapidly determining mixing uniformity. The beneficial effects are as follows:
the method for rapidly determining the mixing uniformity adopts a near infrared spectrum technology, judges the mixing uniformity of a sample on line by using a standard deviation (S) and a variation Coefficient (CV), calculates the standard deviation under each wavelength respectively by taking the absorbance at all wavelength points as an average value, namely S1, S2..S800, and finally obtains the standard deviationCoefficient of variationThe mixing uniformity of the product can be timely and accurately judged by an online test algorithm (standard deviation (S) and Coefficient of Variation (CV)), whether the trends of the standard deviation and the coefficient of variation are consistent, and meanwhile, the near infrared spectrum analysis technology has the advantages of convenient, efficient and accurate analysis of samples, no damage to the samples, no consumption of chemical reagents, no environmental pollution and the like, and can be usedThe mixing endpoint can be determined from a trend analysis of the uniformity of the sample mixture.
Drawings
FIG. 1 is a flow chart of the mixing uniformity measurement of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment one:
as shown in fig. 1, the embodiment of the invention provides a method for rapidly determining mixing uniformity, which is characterized by comprising the following specific steps:
s1, sampling and collecting an original sample before measurement;
s2, collecting near infrared spectrum data of a sample through a near infrared spectrum instrument;
s3, averaging the absorbance of all the collected sample wavelength points;
s4, respectively calculating the difference between the absorbance and the average value of each sample wavelength, namely S1, S2..S 800;
s5, calculating the total standard deviation s=adding the standard deviations at all sample wavelengths (S1, S2..s800), and dividing by the total number of wavelengths (801), i.e.
S6, calculating a variation coefficient CV=dividing the whole standard deviation S by the sample mean X and multiplying by 100%, namely
S7, analyzing the uniformity of samples at different times through an online test algorithm;
s8, whether the standard deviation and the variation coefficient have the same trend or not is judged through an online test algorithm (standard deviation (S) and variation Coefficient (CV)), so that the mixing uniformity of the product can be timely and accurately judged.
Comparative example:
the method for measuring the feed mixing uniformity based on the national standard GB/T5918-2008 comprises the following specific steps:
s1, sample preparation: preparing a feed sample according to a relevant standard, so as to ensure that the sample can represent the whole batch of feed;
s2, dividing the sample: dividing the sample into a plurality of sub-samples, and ensuring that the quality of each sub-sample is equal, usually by using a mechanical divider or a manual sampling mode;
s3, analyzing a subsamples: each sub-sample is analyzed, typically by chemical or physical analysis methods, such as measuring moisture content, particle size distribution, nutrient composition, etc.;
s4, calculating indexes: according to specific evaluation indexes, calculating the difference between measured values of all sub-samples, wherein the indexes commonly used in national standards are variation coefficients;
s5, evaluating results: judging the mixing uniformity of the feed sample according to the calculated index, if the index value is lower than a specific threshold value, indicating that the mixing uniformity of the feed is good, otherwise, if the index value is higher than the threshold value, indicating that the mixing uniformity of the feed is poor:
the results of the mixing effect and time comparison table measured in the above examples and comparative examples are shown in the following table:
| examples | Uniformity of mixture (%) | Time(s) |
| Example 1 | 98.4％ | 30 |
| Comparative example | 93.6％ | 75 |
In summary, the invention judges whether the standard deviation and the variation coefficient have the same trend through an online test algorithm, can judge the mixing uniformity of products timely and accurately, can measure the uniformity of different products, and can further protect the environment without damaging samples and consuming chemical reagents by adopting an infrared spectrum analysis technology.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A method for rapidly determining the uniformity of mixing, comprising the steps of:
s1, sampling and collecting an original sample before measurement;
s2, collecting near infrared spectrum data of a sample through a near infrared spectrum instrument;
s3, averaging the absorbance of all the collected sample wavelength points;
s4, respectively calculating the difference between the absorbance and the average value of each sample wavelength, namely S1, S2..S 800;
s5, calculating the total standard deviation s=adding the standard deviations at all sample wavelengths (S1, S2..s800), and dividing by the total number of wavelengths (801), i.e.
S6, calculating a variation coefficient CV=dividing the whole standard deviation S by the sample mean X and multiplying by 100%, namely
S7, analyzing the uniformity of samples at different times through an online test algorithm;
s8, whether the standard deviation and the variation coefficient have the same trend or not is judged through an online test algorithm (standard deviation (S) and variation Coefficient (CV)), so that the mixing uniformity of the product can be timely and accurately judged.
2. The method for rapidly determining the uniformity of mixing according to claim 1, wherein: the original sample sampling device in the step S1 is an automatic rapid sample concentrator.
3. The method for rapidly determining the uniformity of mixing according to claim 1, wherein: the S2 near infrared spectrometer is AvaSpec CompactLine series spectrometer, the spectrum wavelength range of the collected sample is 900-1700nm, and the total number of the collected sample is 801.
4. The method for rapidly determining the uniformity of mixing according to claim 1, wherein: the absorbance calculation formula in the S3 isWherein A represents absorbance, I0 is the light intensity before the light passes through the medium, and I is the light intensity after the light passes through the medium.
5. The method for rapidly determining the uniformity of mixing according to claim 1, wherein: the standard deviation at the wavelength in S4 is the degree of variation of the spectral intensity value at each specific wavelength in the near infrared spectrum data.
6. The method for rapidly determining the uniformity of mixing according to claim 1, wherein: the larger the coefficient of variation in S6, the higher the relative degree of dispersion of the data, and the smaller the coefficient of variation, the lower the relative degree of dispersion of the data.
7. The method for rapidly determining the uniformity of mixing according to claim 1, wherein: the online test algorithm in S7 and S8 is as follows:
input: data set x= { X1, X2,..xn }, cluster number K;
initializing K cluster centers μ1, μ2, μk;
repeating until convergence: for each data point xi, calculating the distance between each data point xi and each cluster center, selecting the nearest cluster center, classifying the data points into the clusters, and updating the cluster center as the average value of the data points of the clusters to which the data points belong;
and (3) outputting: each data point belongs to a cluster.
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| CN202310915355.2A CN116952895A (en) | 2023-07-25 | 2023-07-25 | Method for rapidly determining mixing uniformity |
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