CN107941747A - Device and method based on the MEMS near infrared technologies detection batch mixing uniformity - Google Patents
Device and method based on the MEMS near infrared technologies detection batch mixing uniformity Download PDFInfo
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- CN107941747A CN107941747A CN201810038020.6A CN201810038020A CN107941747A CN 107941747 A CN107941747 A CN 107941747A CN 201810038020 A CN201810038020 A CN 201810038020A CN 107941747 A CN107941747 A CN 107941747A
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- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000005516 engineering process Methods 0.000 title claims abstract description 19
- 238000001514 detection method Methods 0.000 title claims abstract description 18
- 238000002835 absorbance Methods 0.000 claims abstract description 24
- 238000004458 analytical method Methods 0.000 claims abstract description 16
- 238000001228 spectrum Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 8
- 230000003595 spectral effect Effects 0.000 claims abstract description 7
- 239000000523 sample Substances 0.000 claims description 14
- 229910052594 sapphire Inorganic materials 0.000 claims description 8
- 239000010980 sapphire Substances 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000002329 infrared spectrum Methods 0.000 description 6
- 230000008901 benefit Effects 0.000 description 3
- 239000010437 gem Substances 0.000 description 3
- 229910001751 gemstone Inorganic materials 0.000 description 3
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 241001062009 Indigofera Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—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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- General Physics & Mathematics (AREA)
- Immunology (AREA)
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- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
This application discloses a kind of device and method of the near infrared technology detection batch mixing uniformity based on MEMS, belong to batch mixing mixture homogeneity detection technique field, which includes window structure, and the window structure is installed on batch mixing pot sidewall；Near infrared spectrometer based on MEMS, the near infrared spectrometer are installed on the outside of the window structure.Detecting the uniform method of mixing tank batch mixing is：Step 1：The batch mixing in mixing tank will in real time be detected by window structure based on the near infrared spectrometer of MEMS, and continuously carry out spectra collection and obtain spectral variables, and then obtain multiple absorbance As；Step 2：Calculating analysis is carried out to absorbance A；Step 3：Tendency chart is drawn according to analysis result is obtained in step 2；Step 4：Analytic trend figure, judges that material has reached uniform state if the curve of tendency chart is less than uniformity limit value (MBSD value=0.000035).
Description
Technical field
The present invention relates to batch mixing mixture homogeneity detection field, and in particular to the near infrared online detection batch mixing based on MEMS
The device and its detection method of the uniformity.
Background technology
As long as mixed process is the important step of industry solid pharmaceutical preparation production, mixing can be caused if incorporation time is too short not
Uniformly, product quality is influenced；If the long waste it will cause the energy of incorporation time.Based on the above, the prior art detects batch mixing
The method of degree of mixing is to artificially collect several samples in each mixing batch, is detected by quality procedures, the detection method
Generally require consumption longer time and higher expense, it is difficult to which real-time reflection mixed process instantaneous variation trend is simultaneously timely and effective
Ground judges uniformly mixed terminal.
Near infrared spectrum refers to the infrared electromagnetic wave between near-infrared in, its wavelength is 780~2526nm.It is near red
Wai Pu areas are consistent with sum of fundamental frequencies that hydric group in organic molecule (OH, NH, CH) vibrates and the uptake zone of frequency multiplication at different levels, pass through scanning
The near infrared spectrum of sample, can obtain the characteristic information of organic molecule content group in sample.Pass through the near-infrared to sample
The analysis of spectrum, it is possible to achieve the on-line monitoring to the batch mixing uniformity, it is quick, efficient, accurate to have, and it is excellent not destroy sample etc.
Point.
Number of patent application is that an innovation and creation of CN200610114378.X are disclosed in a kind of detection mixed process not
The method of commaterial mixture homogeneity, this method have following steps：The constituent of multi-medicament preparation is mixed in a mixer
Close 10~30 minutes, take out sample in sample plane in a mixer；Samples taken is loaded to the specimen cup of near infrared spectrometer
In, using irreflexive mensuration mode, scanning wave-number range is selected from 11000~4000cm- 1Wave band, in selected wave band
Take multiple scan, scanning times are respectively 8,16,32,64 times, obtain near infrared spectrum data；Using near infrared spectrometer with
The subsidiary Mathematical treatment software of machine, carries out first derivative processing, then using similarity to obtained near infrared spectrum data
Calculated with method, obtain the similarity numerical value between sample；The uniformity of mixing, different positions are evaluated according to similarity numerical value
Put that the similarity of samples taken is higher, illustrate that the ratio of each component in these samples is closer, that is, the uniformity mixed is better.
Although the described method of the patent document make use of degree of mixing of the advanced near infrared spectrometer to batch mixing to a certain extent
It is detected, but the needs being still unavoidable from manually take out sample in a mixer, and analysis is scanned to sample, its skill
Art means more fall behind, and can not break away from the step of manually extracting sample, it is still desirable to longer time and higher expense are consumed,
It is difficult to reflect mixed process instantaneous variation trend in real time and timely and effectively feeds back to mixed process.
The content of the invention
In view of drawbacks described above of the prior art or deficiency, present invention aims at provide a kind of near-infrared based on MEMS
The devices and methods therefor of the technology on-line checking batch mixing uniformity.
According to an aspect of the invention, there is provided a kind of near infrared technology based on MEMS can on-line checking batch mixing it is uniform
The device of degree, the device include window structure, and window structure is installed on batch mixing pot sidewall；Further include the near-infrared based on MEMS
Spectrometer.MEMS technology, that is, microelectromechanical systems, one is integrated into by mechanical component, optical system, driving part, electric-control system
The microsystem of a integral unit.The advantage of the near infrared spectrometer of MEMS is that reliability is high without mechanical displacement means, is repeated
Good, the good anti-vibration insensitive to vibrating and impacting of property.Near infrared spectrometer is installed on the outside of the window structure, near infrared light
The detectable signal of spectrometer probe is through the batch mixing in window structure detection mixing tank.
It is further optimization of the present invention to above-mentioned technical proposal below：
Further, window structure includes ring flange, and eyeglass is connected with the opening in the middle part of ring flange.
Further, the snap fit of ring flange and eyeglass is：Eyeglass is embedded into the opening, and the edge of eyeglass leads to
Flange cover plate compression is crossed, the mode that flange cover plate is connected through a screw thread is fixed on ring flange.
Further, eyeglass is sapphire eyeglass, the eyeglass of window structure use the benefit of sapphire material for：(1) it is blue
Jewel hardness is high, it is possible to prevente effectively from frictional dissipation of the material to eyeglass in mixed process, keeps mirror-smooth transparent；(2) it is blue
Jewel material does not absorb near infrared light, can be completely through, can effectively improve the accuracy and precision of near infrared spectrum.
According to another aspect of the present invention, the side that above device realizes on-line checking batch mixing uniformity function is additionally provided
Method, comprises the following steps：
Step 1：The batch mixing in mixing tank will be examined in real time by window structure based on the near infrared spectrometer of MEMS
Survey, and continuously carry out spectra collection and obtain spectral variables, and then obtain multiple absorbance As；
Step 2：Calculating analysis is carried out to absorbance A；
Step 3：Tendency chart is drawn according to analysis result is obtained in step 2；
Step 4：Analytic trend figure, if the curve of tendency chart is less than uniformity limit value (MBSD value=0.000035)
Reach uniform state.
It is further optimization of the present invention to above-mentioned technical proposal below：
In step 1, the spectral variables that MEMS near infrared technologies carry out spectra collection are the wavelength i and light of batch mixing feedback
Compose number j.
In step 2, absorbance is carried out to need to carry out first differential processing to absorbance A before calculating analysis.
In step 2, the method for absorbance A calculate analysis is：
The first step, the absorbance A of the continuous spectrum of m selection n, and calculate the standard of absorbance A at each wavelength i
Deviation Si, specific formula is:
Second step, tries to achieve last uniformity S, i.e. MBSD values, and specific formula is
In step 3, the drafting principle of tendency chart is：Abscissa variable using the time as tendency chart, uniformity MBSD
It is worth the ordinate variable as tendency chart.
When occurring more stable curve in step 4, on tendency chart, it is uniform to represent batch mixing, and uniformity MBSD values value becomes
Change amplitude is smaller, and it is more uniform to represent batch mixing.
The beneficial effects of the invention are as follows：
1. a kind of exemplary near infrared technology based on MEMS of the present invention can the on-line checking batch mixing uniformity device, pass through
The mutual cooperation of window structure and near infrared spectrometer based on MEMS can realize that detection mixed process instantaneous variation becomes in real time
Gesture simultaneously is timely and effectively judged to be uniformly mixed terminal, it is not necessary to repeatedly extracts sample, substantially increases batch mixing efficiency and save
Financial resources.
2. a kind of exemplary near infrared spectrometer based on MEMS of the present invention, is sensed using the micro spectrometer of high integration
Device module, has the characteristics that reliability is high, reproducible, good anti-vibration 1. without mechanical displacement means；2. equipment volume
It is small, light-weight, complete machine weight 1kg；3. power is very low, only 1W；4. carried out data transmission and equipment using the bluetooth of low-power consumption
Control.Therefore, there is higher cost performance, be very suitable for the on-line monitoring to the batch mixing uniformity.
3rd, the method that a kind of exemplary near-infrared spectrum technique based on MEMS of the present invention realizes the detection batch mixing uniformity, can
Mixing process to be digitized, quantify, visualization so that process operator can be more directly perceived directly to mixing procedure
Uniformity coefficient carries out control, greatly improves batch mixing whole efficiency.
By reading the detailed description made to non-limiting example made with reference to the following drawings, the application's is other
Feature, objects and advantages will become more apparent upon：
Fig. 1 is mixing tank structure diagram；
Fig. 2 is window structure side sectional view；
Fig. 3 is window structure front view；
Fig. 4 is the MBSD Trendline sectional drawings of batch mixing
In figure：1st, mixing tank, 2, window structure, 2-1, flange cover plate, 2-2 ring flanges, 2-3, screw thread, 3, sapphire mirror
Piece.
Specific embodiment
The application is described in further detail with reference to the accompanying drawings and examples.It is understood that this place is retouched
The specific embodiment stated is used only for explaining related invention, rather than the restriction to the invention.It also should be noted that in order to
It illustrate only easy to describe, in attached drawing with inventing relevant part.
It should be noted that in the case where there is no conflict, the feature in embodiment and embodiment in the application can phase
Mutually combination.Describe the application in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
Embodiment 1
As shown in Fig. 1 to Fig. 3, the present embodiment to provide a kind of near infrared technology on-line checking batch mixing based on MEMS equal
The device of evenness, the device include window structure 2, and window structure 2 is installed on 1 side wall of mixing tank；Further include based on MEMS's
Near infrared spectrometer, near infrared spectrometer are installed on the outside of window structure 2, and the detectable signal of near infrared spectrometer probe is saturating
Cross the batch mixing in the detection of window structure 2 mixing tank 1.Window structure 2 includes ring flange 2-2, the opening in the middle part of ring flange 2-2
Inside it is connected with eyeglass.The snap fit of ring flange 2-2 and eyeglass is：Eyeglass is embedded into the opening, and the edge of eyeglass leads to
Flange cover plate 2-1 compressions are crossed, flange cover plate 2-1 is fixed on ring flange 2-2 by way of screw thread 2-3 is connected.Eyeglass is indigo plant
Gemstone lens 3.
The present embodiment additionally provides the method on the above-mentioned material pot on-line checking batch mixing uniformity, including following step
Suddenly：
Step 1：The batch mixing in mixing tank will be examined in real time by window structure based on the near infrared spectrometer of MEMS
Survey, and continuously carry out spectra collection and obtain spectral variables, and then obtain multiple absorbance As；
Step 2：Calculating analysis is carried out to absorbance A；
Step 3：Tendency chart is drawn according to analysis result is obtained in step 2；
Step 4：Analytic trend figure, if the curve of tendency chart is consistently less than uniformity limit value (MBSD value=0.000035)
Then judge that material has reached uniform state.
Further：
In step 1, the spectral variables that MEMS near infrared technologies carry out spectra collection are the wavelength i and light of batch mixing feedback
Compose number j.
In step 2, absorbance is carried out to need to carry out first differential processing to absorbance A before calculating analysis.
In step 2, the method for absorbance A calculate analysis is：
The first step, the absorbance A of the continuous spectrum of m selection n, and calculate the standard of absorbance A at each wavelength i
Deviation Si, specific formula is:
Second step, tries to achieve last uniformity S, i.e. MBSD values, and specific formula is
In step 3, the drafting principle of tendency chart is：Abscissa variable using the time as tendency chart, uniformity MBSD
It is worth the ordinate variable as tendency chart.
With reference to shown in Fig. 4, if batch mixing has reached uniform state, then occur that n continuous absorbances are very close
Situation, show occur more stable smooth MBSD curves on tendency chart, at this time MBSD (MBSD values=
0.000035) value reaches minimum.MBSD values are only used for judging mixture homogeneity, and the more low then mixture homogeneity of MBSD values is better.
Based on the near-infrared beam splitting system of MEMS technology manufacture, i.e. MEMS near infrared spectrometers, near infrared light can be produced
Spectrum.Sapphire form is installed, MEMS near infrared spectrometers connect whole mixing process by the form online on batch mixer
Continuous spectra collection, and spectrum is analyzed in real time online.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.People in the art
Member should be appreciated that invention scope involved in the application, however it is not limited to the technology that the particular combination of above-mentioned technical characteristic forms
Scheme, while should also cover in the case where not departing from the inventive concept, carried out by above-mentioned technical characteristic or its equivalent feature
The other technical solutions for being combined and being formed.Such as features described above has similar work(with (but not limited to) disclosed herein
The technical solution that the technical characteristic of energy is replaced mutually and formed.
Claims (10)
1. a kind of device based on the MEMS near infrared technologies detection batch mixing uniformity, it is characterised in that the device includes
Window structure, the window structure are installed on batch mixing pot sidewall；
Near infrared spectrometer based on MEMS, the near infrared spectrometer are installed on the outside of the window structure, the near-infrared
The detectable signal of spectrometer probe is through the batch mixing in window structure detection mixing tank.
2. a kind of device based on the MEMS near infrared technologies detection batch mixing uniformity according to claim 1, its feature exist
Include ring flange in, the window structure, sapphire eyeglass is connected with the opening in the middle part of the ring flange.
3. a kind of device based on the MEMS near infrared technologies detection batch mixing uniformity according to claim 2, its feature exist
In the snap fit of ring flange and the sapphire eyeglass is：Eyeglass is embedded into the opening, the side of the sapphire eyeglass
Compressed at by flange cover plate, the mode that the flange cover plate is connected through a screw thread is fixed on the ring flange.
4. a kind of device based on the MEMS near infrared technologies detection batch mixing uniformity according to claim 3, its feature exist
In the eyeglass is sapphire eyeglass.
5. a kind of method of device on-line checking batch mixing uniformity as described in Claims 1 to 4, it is characterised in that including with
Lower step：
Step 1：The batch mixing in mixing tank will be detected in real time by window structure based on the near infrared spectrometer of MEMS,
And continuously carry out spectra collection and obtain spectral variables, and then obtain multiple absorbance As；
Step 2：Calculating analysis is carried out to absorbance A；
Step 3：Tendency chart is drawn according to analysis result is obtained in step 2；
Step 4：Analytic trend figure, judges thing if the curve of tendency chart is less than uniformity limit value (MBSD value=0.000035)
Material judges that material has reached uniform state.
6. the method for the on-line checking batch mixing uniformity according to claim 5, it is characterised in that in the step one
In, the spectral variables that MEMS near infrared technologies carry out spectra collection are the wavelength i and spectrum number j of batch mixing feedback.
7. the method for the on-line checking batch mixing uniformity according to claim 6, it is characterised in that in the step two
In, absorbance is carried out to need to carry out first differential processing to absorbance A before calculating analysis.
8. the method for the on-line checking batch mixing uniformity according to claim 7, it is characterised in that in the step two
In, the method for absorbance A calculate analysis is：
The first step, the absorbance A of the continuous spectrum of m selection n, and calculate the standard deviation of absorbance A at each wavelength i
Si, specific formula is:
Second step, tries to achieve last uniformity S, i.e. MBSD values, and specific formula is
9. the method for the on-line checking batch mixing uniformity according to claim 8, it is characterised in that in the step 3,
The drafting principle of tendency chart is：Abscissa variable using the time as tendency chart, uniformity S become as the ordinate of tendency chart
Amount.
10. the method for the on-line checking batch mixing uniformity according to claim 9, it is characterised in that in the step four
In, MBSD values are lower on tendency chart, represent that batch mixing is more uniform, and uniformity MBSD value amplitudes of variation are smaller, and it is more equal to represent batch mixing
It is even.
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Cited By (7)
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| CN109738342A (en) * | 2019-03-18 | 2019-05-10 | 山东金璋隆祥智能科技有限责任公司 | A method of size distribution is detected based on near-infrared spectrum technique |
| CN110865048A (en) * | 2019-12-09 | 2020-03-06 | 西华大学 | Nondestructive testing method for monitoring mixing uniformity of ingredients |
| CN112240876A (en) * | 2019-07-17 | 2021-01-19 | 华东理工大学 | Method for detecting fermentation process parameters in real time based on near infrared |
| WO2021017745A1 (en) * | 2019-07-26 | 2021-02-04 | 中国农业大学 | Material uniformity detection device and method |
| CN113655019A (en) * | 2021-08-10 | 2021-11-16 | 南京富岛信息工程有限公司 | Oil mixing interface detection method for crude oil in pipeline transportation |
| CN114166829A (en) * | 2021-12-08 | 2022-03-11 | 华中科技大学鄂州工业技术研究院 | Slurry uniformity detection system and method |
| CN114471275A (en) * | 2021-12-30 | 2022-05-13 | 西安近代化学研究所 | Mixing roller, medicine mixing detection equipment, medicine mixing detection method and application |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109738342A (en) * | 2019-03-18 | 2019-05-10 | 山东金璋隆祥智能科技有限责任公司 | A method of size distribution is detected based on near-infrared spectrum technique |
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| WO2021017745A1 (en) * | 2019-07-26 | 2021-02-04 | 中国农业大学 | Material uniformity detection device and method |
| US11719623B2 (en) | 2019-07-26 | 2023-08-08 | China Agricultural University | Slurry material uniformity detection device and detection method |
| CN110865048A (en) * | 2019-12-09 | 2020-03-06 | 西华大学 | Nondestructive testing method for monitoring mixing uniformity of ingredients |
| CN113655019A (en) * | 2021-08-10 | 2021-11-16 | 南京富岛信息工程有限公司 | Oil mixing interface detection method for crude oil in pipeline transportation |
| CN113655019B (en) * | 2021-08-10 | 2024-04-26 | 南京富岛信息工程有限公司 | Method for detecting oil mixing interface of crude oil conveyed by pipeline |
| CN114166829A (en) * | 2021-12-08 | 2022-03-11 | 华中科技大学鄂州工业技术研究院 | Slurry uniformity detection system and method |
| CN114166829B (en) * | 2021-12-08 | 2023-09-19 | 华中科技大学鄂州工业技术研究院 | Slurry uniformity detection system and method |
| CN114471275A (en) * | 2021-12-30 | 2022-05-13 | 西安近代化学研究所 | Mixing roller, medicine mixing detection equipment, medicine mixing detection method and application |
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Application publication date: 20180420 |